The Reversible Formation of a Single-Bonded (C60-)2 Dimer in Ionic Charge Transfer Complex: Cp*2Cr.C60(C6H4Cl2)2. The Molecular Structure of (C60-)2
Dmitri V. Konarev; Salavat S. Khasanov; Akihiro Otsuka; Gunzi Saito; Journal of the American Chemical Society 124 (2002) 8520–8521; doi:10.1021/ja0202614

data_4114959
_publ_section_title
;
 The Reversible Formation of a Single-Bonded (C60-)2 Dimer in Ionic Charge
 Transfer Complex: Cp*2Cr.C60(C6H4Cl2)2. The Molecular Structure of
 (C60-)2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8520
_journal_page_last               8521
_journal_paper_doi               10.1021/ja0202614
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         '2(C120 2-), 4(C20 H30 Cr1 1+), 8(C6 H4 Cl2)'
_chemical_formula_sum            'C368 H152 Cl16 Cr4'
_chemical_formula_weight         5348.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.387(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.793(1)
_cell_length_b                   20.785(1)
_cell_length_c                   24.747(1)
_cell_measurement_reflns_used    34678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.06
_cell_volume                     11247.7(9)
_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      100(2)
_diffrn_detector_area_resol_mean 0.08
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.865
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            60455
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.8051
_exptl_absorpt_correction_T_min  0.8051
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5456
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.059(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4593
_refine_ls_number_reflns         23077
_refine_ls_number_restraints     1899
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.463
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+10.4268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                15377
_reflns_number_total             23077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0202614.cif
_cod_data_source_block           s22p3
_cod_database_code               4114959