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_4306897
_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
'(C70)4, C44 H28 MN N4, (C7 H15 N2)4, (C6 H4 CL2)6, (C7 H5 N)4.8'
_chemical_formula_sum            'C421.6 H136 Cl12 Mn N16.8'
_chemical_formula_weight         5916.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.606(3)
_cell_angle_beta                 81.629(3)
_cell_angle_gamma                63.610(3)
_cell_formula_units_Z            1
_cell_length_a                   19.1170(10)
_cell_length_b                   19.5660(10)
_cell_length_c                   20.7310(10)
_cell_measurement_reflns_used    78878
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6419.7(6)
_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      90(2)
_diffrn_detector_area_resol_mean 0.08
_diffrn_measured_fraction_theta_full 0.872
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type  'MAC_Science Image Plate diffractometer'
_diffrn_measurement_method       'oscillation pattern reflections 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  0.06
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25574
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.256
_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    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3012
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2721
_refine_ls_number_reflns         25574
_refine_ls_number_restraints     1487
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+7.2534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                19154
_reflns_number_total             25574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0611138si20060620_091238.cif
_cod_data_source_block           sk23
_cod_original_formula_sum        'C421.60 H136 Cl12 Mn1 N16.80'
_cod_database_code               4306897