Weak Ferromagnetism and Strong Spin-Spin Interaction Mediated by the Mixed-Valence Ethynyltetrathiafulvalene-Type Ligand
Junichi Nishijo; Ken Judai; Nobuyuki Nishi; Inorganic Chemistry 50 (2011) 3464–3470; doi:10.1021/ic102384s

data_4324862
_publ_section_title
;
 Weak Ferromagnetism and Strong Spin-Spin Interaction Mediated by the
 Mixed-Valence Ethynyltetrathiafulvalene-Type Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3464
_journal_page_last               3470
_journal_paper_doi               10.1021/ic102384s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C33 H38 Cr F3 N4 O3 S13'
_chemical_formula_weight         1064.54
_chemical_name_common            '[CrCyclam(C2MeEDT)2]OTf'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.959(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8733(18)
_cell_length_b                   11.4891(13)
_cell_length_c                   22.710(3)
_cell_measurement_reflns_used    18002
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      30.5601
_cell_measurement_theta_min      1.4563
_cell_volume                     4392.0(9)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (M. C. Burla et al.)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 83.6000
_diffrn_measured_fraction_theta_max 30.5601
_diffrn_measurement_device       'Mercury (2x2 bin mode)'
_diffrn_measurement_device_type  'Rigaku AFC7R with CCD detector'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.1172
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42828
_diffrn_reflns_theta_full        30.5601
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.9266
_exptl_absorpt_correction_T_min  0.7600
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.957
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.318
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         17441
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.1471
_refine_ls_shift/su_max          0.163
_refine_ls_shift/su_mean         0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1870P)^2^+166.6476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3903
_refine_ls_wR_factor_ref         0.3965
_reflns_number_gt                14071
_reflns_number_total             17441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102384s_si_001_1.cif
_cod_data_source_block           '[CrCyclam(C2MeEDT)2]OTf'
_cod_original_cell_volume        4392.1(9)
_cod_original_formula_sum        'C33 H38 Cr1 F3 N4 O3 S13'
_cod_database_code               4324862