 
data_juf59
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             C60.2tetrachloroethene
_chemical_melting_point           ?
_chemical_formula_moiety          'C60, 2(C2 Cl4)'
_chemical_formula_sum
 'C64 Cl8' 
_chemical_formula_weight          1052.24

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            12
_space_group_name_H-M_alt         'C 2/m'
_space_group_name_Hall            '-C 2y'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'
 
_cell_length_a                    16.0981(12)
_cell_length_b                    11.4891(9)
_cell_length_c                    10.2043(8)
_cell_angle_alpha                 90
_cell_angle_beta                  102.0260(11)
_cell_angle_gamma                 90
_cell_volume                      1845.9(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     90(2)
_cell_measurement_reflns_used     5291
_cell_measurement_theta_min       2.6
_cell_measurement_theta_max       27.5
 
_exptl_crystal_description        shard
_exptl_crystal_colour             black
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.893          
_exptl_crystal_F_000              1040
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.320
_exptl_crystal_size_mid           0.180
_exptl_crystal_size_min           0.070
_exptl_absorpt_coefficient_mu     0.667
_shelx_estimated_absorpt_T_min    0.815
_shelx_estimated_absorpt_T_max    0.955
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.522
_exptl_absorpt_correction_T_max   0.746
_exptl_absorpt_process_details    'SADABS (Sheldrick, 2016)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       90(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'
_diffrn_measurement_device_type   'Bruker ApexII'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  8.3
_diffrn_reflns_number             10499
_diffrn_reflns_av_unetI/netI      0.0218
_diffrn_reflns_av_R_equivalents   0.0299
_diffrn_reflns_limit_h_min        -20
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.587
_diffrn_reflns_theta_max          27.536
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              2223
_reflns_number_gt                 2000
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Apex2 (Bruker, 2008)'
_computing_cell_refinement        'SAINT (Bruker v8.38A, 2017)'
_computing_data_reduction         'SAINT (Bruker v8.38A, 2017)'
_computing_structure_solution     'SHELXS, (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details           
;The solvate C2Cl4 is disordered by symmetry
with respect to the crystallographic
mirror plane (Wyckoff position i).
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0652P)²+3.6605P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2223
_refine_ls_number_parameters      178
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0423
_refine_ls_R_factor_gt            0.0384
_refine_ls_wR_factor_ref          0.1117
_refine_ls_wR_factor_gt           0.1086
_refine_ls_goodness_of_fit_ref    1.040
_refine_ls_restrained_S_all       1.040
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.36405(11) 0.70012(17) 0.29505(19) 0.0185(4) Uani 1 1 d . . . . .
C2 C 0.32993(11) 0.70019(17) 0.41597(19) 0.0180(4) Uani 1 1 d . . . . .
C3 C 0.28818(10) 0.60219(17) 0.44968(18) 0.0180(4) Uani 1 1 d . . . . .
C4 C 0.27894(15) 0.500000 0.3643(3) 0.0176(5) Uani 1 2 d S T P . .
C5 C 0.31160(15) 0.500000 0.2487(3) 0.0176(5) Uani 1 2 d S T P . .
C6 C 0.35501(11) 0.60256(17) 0.21342(17) 0.0178(4) Uani 1 1 d . . . . .
C7 C 0.42526(11) 0.56314(18) 0.15544(17) 0.0184(4) Uani 1 1 d . . . . .
C8 C 0.50194(11) 0.62353(18) 0.18253(17) 0.0192(4) Uani 1 1 d . . . . .
C9 C 0.51106(11) 0.72559(17) 0.26808(19) 0.0195(4) Uani 1 1 d . . . . .
C10 C 0.44385(12) 0.76351(17) 0.32309(19) 0.0195(4) Uani 1 1 d . . . . .
C11 C 0.45884(12) 0.80272(16) 0.4611(2) 0.0199(4) Uani 1 1 d . . . . .
C12 C 0.38870(11) 0.76328(16) 0.51895(19) 0.0195(4) Uani 1 1 d . . . . .
C13 C 0.40305(11) 0.72559(17) 0.65111(19) 0.0193(4) Uani 1 1 d . . . . .
C14 C 0.35967(11) 0.62353(18) 0.68658(18) 0.0192(4) Uani 1 1 d . . . . .
C15 C 0.30330(10) 0.56319(17) 0.58803(18) 0.0185(4) Uani 1 1 d . . . . .
C16 C 0.41821(11) 0.56064(18) 0.78934(18) 0.0196(4) Uani 1 1 d . . . . .
Cl1 Cl 0.14105(3) 0.68610(4) 0.03441(5) 0.02793(17) Uani 1 1 d . . . . .
Cl2 Cl 0.06652(4) 0.500000 0.18385(7) 0.02360(18) Uani 1 2 d S T P . .
Cl3 Cl 0.21192(6) 0.500000 -0.12153(8) 0.0427(2) Uani 1 2 d S T P . .
C17 C 0.1229(2) 0.5383(3) 0.0650(4) 0.0172(7) Uani 0.5 1 d . . P . .
C18 C 0.1556(2) 0.4554(4) -0.0014(4) 0.0202(7) Uani 0.5 1 d . . P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C6 1.386(3) . ?
C1 C2 1.451(3) . ?
C1 C10 1.452(3) . ?
C2 C3 1.391(3) . ?
C2 C12 1.453(3) . ?
C3 C4 1.451(2) . ?
C3 C15 1.453(3) . ?
C4 C5 1.388(4) . ?
C5 C6 1.453(2) . ?
C5 C6 1.453(2) 6_565 ?
C6 C7 1.454(2) . ?
C7 C8 1.393(3) . ?
C7 C7 1.451(4) 6_565 ?
C8 C16 1.450(3) 2_656 ?
C8 C9 1.451(3) . ?
C9 C10 1.389(3) . ?
C9 C13 1.455(2) 2_656 ?
C10 C11 1.451(3) . ?
C11 C11 1.396(4) 2_656 ?
C11 C12 1.451(3) . ?
C12 C13 1.389(3) . ?
C13 C14 1.449(3) . ?
C14 C15 1.391(3) . ?
C14 C16 1.448(3) . ?
C15 C15 1.452(4) 6_565 ?
C16 C16 1.393(4) 6_565 ?
Cl1 C18 1.693(4) 6_565 ?
Cl1 C17 1.762(4) . ?
Cl2 C17 1.717(4) . ?
Cl2 C17 1.717(4) 6_565 ?
Cl3 C18 1.747(4) . ?
Cl3 C18 1.747(4) 6_565 ?
C17 C17 0.881(7) 6_565 ?
C17 C18 0.943(5) 6_565 ?
C17 C18 1.338(6) . ?
C18 C18 1.025(8) 6_565 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C6 C1 C2 120.03(17) . . ?
C6 C1 C10 120.12(17) . . ?
C2 C1 C10 107.95(16) . . ?
C3 C2 C1 119.86(17) . . ?
C3 C2 C12 120.03(17) . . ?
C1 C2 C12 108.09(16) . . ?
C2 C3 C4 120.04(17) . . ?
C2 C3 C15 119.89(17) . . ?
C4 C3 C15 108.04(17) . . ?
C5 C4 C3 120.06(13) . . ?
C5 C4 C3 120.06(13) . 6_565 ?
C3 C4 C3 108.0(2) . 6_565 ?
C4 C5 C6 119.84(13) . . ?
C4 C5 C6 119.84(13) . 6_565 ?
C6 C5 C6 108.4(2) . 6_565 ?
C1 C6 C5 120.17(17) . . ?
C1 C6 C7 120.23(17) . . ?
C5 C6 C7 107.66(17) . . ?
C8 C7 C7 119.88(11) . 6_565 ?
C8 C7 C6 119.78(18) . . ?
C7 C7 C6 108.15(11) 6_565 . ?
C7 C8 C16 120.23(18) . 2_656 ?
C7 C8 C9 119.76(16) . . ?
C16 C8 C9 108.01(16) 2_656 . ?
C10 C9 C8 120.47(17) . . ?
C10 C9 C13 119.96(18) . 2_656 ?
C8 C9 C13 107.82(16) . 2_656 ?
C9 C10 C11 120.27(17) . . ?
C9 C10 C1 119.65(18) . . ?
C11 C10 C1 107.96(16) . . ?
C11 C11 C10 119.9(2) 2_656 . ?
C11 C11 C12 119.8(2) 2_656 . ?
C10 C11 C12 108.16(16) . . ?
C13 C12 C11 120.39(16) . . ?
C13 C12 C2 119.88(18) . . ?
C11 C12 C2 107.84(16) . . ?
C12 C13 C14 120.23(17) . . ?
C12 C13 C9 119.76(17) . 2_656 ?
C14 C13 C9 108.01(16) . 2_656 ?
C15 C14 C16 120.19(18) . . ?
C15 C14 C13 119.90(17) . . ?
C16 C14 C13 108.04(16) . . ?
C14 C15 C15 119.89(11) . 6_565 ?
C14 C15 C3 120.06(17) . . ?
C15 C15 C3 107.97(11) 6_565 . ?
C16 C16 C14 119.92(11) 6_565 . ?
C16 C16 C8 119.89(11) 6_565 2_656 ?
C14 C16 C8 108.12(17) . 2_656 ?
C18 Cl1 C17 31.60(18) 6_565 . ?
C17 Cl2 C17 29.7(3) . 6_565 ?
C18 Cl3 C18 34.1(3) . 6_565 ?
C17 C17 C18 94.4(3) 6_565 6_565 ?
C17 C17 C18 44.6(2) 6_565 . ?
C18 C17 C18 49.8(4) 6_565 . ?
C17 C17 Cl2 75.14(13) 6_565 . ?
C18 C17 Cl2 169.5(4) 6_565 . ?
C18 C17 Cl2 119.8(3) . . ?
C17 C17 Cl1 164.54(13) 6_565 . ?
C18 C17 Cl1 70.2(3) 6_565 . ?
C18 C17 Cl1 119.9(3) . . ?
Cl2 C17 Cl1 120.2(2) . . ?
C17 C18 C18 85.6(3) 6_565 6_565 ?
C17 C18 C17 41.0(4) 6_565 . ?
C18 C18 C17 44.6(2) 6_565 . ?
C17 C18 Cl1 78.2(3) 6_565 6_565 ?
C18 C18 Cl1 163.76(14) 6_565 6_565 ?
C17 C18 Cl1 119.2(3) . 6_565 ?
C17 C18 Cl3 158.5(4) 6_565 . ?
C18 C18 Cl3 72.95(13) 6_565 . ?
C17 C18 Cl3 117.6(3) . . ?
Cl1 C18 Cl3 123.3(2) 6_565 . ?
 
_refine_diff_density_max    0.446
_refine_diff_density_min   -0.429
_refine_diff_density_rms    0.077



