Ferro- and Antiferromagnetic Coupling Switch Accompanied by Twist Deformation around the Copper(II) and Nitroxide Coordination Bond
Atsushi Okazawa; Daisuke Hashizume; Takayuki Ishida; Journal of the American Chemical Society 132 (2010) 11516–11524; doi:10.1021/ja102163d

data_4102861
_publ_contact_author_address
;
    Department of Applied Physics and Chemistry, The University of 
    Electro-Communications, Chofu, Tokyo 182-8585, Japan
;
_publ_contact_author_email       ' ishi@pc.uec.ac.jp '
_publ_contact_author_fax         ' +81-42-443-5501 '
_publ_contact_author_name        'Takayuki Ishida'
_publ_contact_author_phone       ' +81-42-443-5490 '
_publ_section_title
;
 Ferro- and Antiferromagnetic Coupling Switch Accompanied by Twist
 Deformation around the Copper(II) and Nitroxide Coordination Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11516
_journal_page_last               11524
_journal_paper_doi               10.1021/ja102163d
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C36 H52 Cu2 N8 O4, 2(B F4)'
_chemical_formula_sum            'C36 H52 B2 Cu2 F8 N8 O4'
_chemical_formula_weight         961.56
_chemical_melting_point          448(2)
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.342(1)
_cell_length_b                   17.360(1)
_cell_length_c                   12.514(1)
_cell_measurement_reflns_used    257087
_cell_measurement_temperature    50
_cell_measurement_theta_max      43.34
_cell_measurement_theta_min      1.37
_cell_volume                     4201.9(5)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'DIP Xpress'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      50
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'MacScience Vacuum Camera'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'SPring-8 BL02B1 bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.61792
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            178714
_diffrn_reflns_theta_full        43.34
_diffrn_reflns_theta_max         43.34
_diffrn_reflns_theta_min         2.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.77508
_exptl_absorpt_correction_T_min  0.71262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   MULABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.473
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         23978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0470P)^2^+1.8676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                17579
_reflns_number_total             23978
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja102163d_si_002.cif
_cod_data_source_block           '_[Cu(2pyNO-)(2pyNO.)]2(BF4-)2_50K'
_cod_database_code               4102861