Formation of Antiferromagnetically Coupled C60.- and Diamagnetic (C70-)2 Dimers in Ionic Complexes of Fullerenes with (MDABCO+)2.MIITPP (M = Zn, Co, Mn, and Fe) Assemblies
Dmitri V. Konarev; Salavat S. Khasanov; Akihiro Otsuka; Gunzi Saito; Rimma N. Lyubovskaya; Inorganic Chemistry 46 (2007) 2261–2271; doi:10.1021/ic0611138

data_4306896
_publ_contact_author_address
;
Devision of chemistry, Graduate School of Science,
Kyoto University, Sakyo-ku, Kyoto 606-8502, Japan
;
_publ_contact_author_email       saito@kuchem.kyoto-u.ac.jp
_publ_contact_author_name        'Professor G. Saito'
_publ_section_title
;
Formation of Antiferromagnetically Coupled C60.- and Diamagnetic
(C70-)2 Dimers in Ionic Complexes of Fullerenes with (MDABCO+)2.MIITPP (M =
Zn, Co, Mn, and Fe) Assemblies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2261
_journal_page_last               2271
_journal_paper_doi               10.1021/ic0611138
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'(C60)2, C44 H28 Mn N4, (C7 H15 N2)2, (C6 H4 CL2)4.2, (C7 H5 N)1.8'
_chemical_formula_sum            'C215.8 H83.8 Cl8.4 Mn N9.8'
_chemical_formula_weight         3166.25
_chemical_name_systematic
;
 ?
;
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0250(10)
_cell_length_b                   25.9500(10)
_cell_length_c                   25.938(2)
_cell_measurement_reflns_used    81586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     13478.6(13)
_computing_cell_refinement       MAC-DENZO
_computing_data_collection       MAC-DENZO
_computing_data_reduction        MAC-DENZO
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.08
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'MAC_Science Image Plate diffractometer'
_diffrn_measurement_method       'oscillation pattern raflections integration'
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32062
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
reflections integration procedure incorporates scaling procedures that takes
into account absorption corrections too; in case of low absorption crystals it 
works well
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6460
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         12559
_refine_ls_number_restraints     275
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+9.5934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                8673
_reflns_number_total             12559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0611138si20060620_091219.cif
_cod_data_source_block           sk151c
_cod_original_formula_sum        'C215.80 H83.80 Cl8.40 Mn N9.80'
_cod_database_code               4306896