An order‒disorder phase transition in the structure of C~60~·4benzene
Olmstead, Marilyn M.; Balch, Alan L.; Lee, Hon Man; Acta Crystallographica Section B 68 (2012) 66–70; doi:10.1107/S0108768111046593

data_2105067
_publ_section_title
;
 An order--disorder phase transition in the structure of
 C~60~&#x00B7;4benzene
;
_journal_coeditor_code           RY5039
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              66
_journal_page_last               70
_journal_paper_doi               10.1107/S0108768111046593
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C60, 4(C6 H6)'
_chemical_formula_sum            'C84 H24'
_chemical_formula_weight         1033.03
_chemical_name_common            C~60~^.^4benzene
_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                65.377(3)
_cell_angle_beta                 88.098(3)
_cell_angle_gamma                74.812(2)
_cell_formula_units_Z            4
_cell_length_a                   9.8842(12)
_cell_length_b                   15.0159(19)
_cell_length_c                   34.691(4)
_cell_measurement_reflns_used    788
_cell_measurement_temperature    13(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      2.6
_cell_volume                     4500.2(10)
_computing_cell_refinement       'SAINT 6.36A (Bruker, 2002)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36A (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      13(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_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  0.055
_diffrn_reflns_av_sigmaI/netI    0.2441
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            20798
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.225
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1501
_refine_ls_number_reflns         20479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.710
_refine_ls_R_factor_all          0.2018
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0142P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                6542
_reflns_number_total             20479
_reflns_threshold_expression     I>2\s(I)
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_cod_database_fobs_code          2105067