Synthesis and Crystal Structure of Ionic Multicomponent Complex: {[CrI(PhH)2].+}2[CoIITPP(C60(CN)2)]-[C60(CN)2].-.3(o-C6H4Cl2) Containing C60(CN)2.- Radical Anion and σ-Bonded Diamagnetic CoIITPP(C60(CN)2)- Anion
Dmitry V. Konarev; Salavat S. Khasanov; Akihiro Otsuka; Yukihiro Yoshida; Gunzi Saito; Journal of the American Chemical Society 124 (2002) 7648–7649; doi:10.1021/ja0203667

data_4114922
_publ_section_title
;
 Synthesis and Crystal Structure of Ionic Multicomponent Complex:
 {[CrI(PhH)2].+}2[CoIITPP(C60(CN)2)]-[C60(CN)2].-.3(o-C6H4Cl2) Containing
 C60(CN)2.- Radical Anion and \s-Bonded Diamagnetic CoIITPP(C60(CN)2)-
 Anion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7648
_journal_page_last               7649
_journal_paper_doi               10.1021/ja0203667
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety
'(C62 N2 1-)4, (C12 H12 Cr1 1+)4, 2(C44 H28 N4 Co1), 6(C6 H4 Cl2)'
_chemical_formula_sum            'C420 H128 Cl12 Co2 Cr4 N16'
_chemical_formula_weight         6148.64
_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                92.300(10)
_cell_angle_beta                 100.890(10)
_cell_angle_gamma                103.460(10)
_cell_formula_units_Z            1
_cell_length_a                   13.9670(10)
_cell_length_b                   15.9280(10)
_cell_length_c                   30.3320(10)
_cell_measurement_temperature    120(2)
_cell_volume                     6419.3(8)
_computing_cell_refinement       MAC-DENZO
_computing_data_collection       MAC-DENZO
_computing_data_reduction        MAC-DENZO
_computing_molecular_graphics    ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 0.08
_diffrn_measured_fraction_theta_full 0.774
_diffrn_measured_fraction_theta_max 0.774
_diffrn_measurement_device_type  'MAC-Science Image Plate'
_diffrn_measurement_method
'Image plate 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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            37757
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.9341
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
   no absorbtion correction was applied, for
   the long axis of the sample was approximately
   perpendicular to X-ray beam, so T_min to
   T_max ratio was about 0.95
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3114
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.600
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2383
_refine_ls_number_reflns         22474
_refine_ls_number_restraints     818
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+8.9887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1882
_reflns_number_gt                17869
_reflns_number_total             22474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0203667.cif
_cod_data_source_block           s18b
_cod_original_cell_volume        6419.3(6)
_cod_database_code               4114922