Crippling the C70 Fullerene: Non-Classical C68Cl26(OH)2 and C68Cl25(OH)3 with Three Heptagons and Only Fused Pentagons via Chlorination-Promoted Skeletal Transformations
Brotsman, Victor A.; Ioffe, Ilya N.; Troyanov, Sergey I.; Chemical Communications  (2022) –; doi:10.1039/D2CC01719A

data_7130129
_publ_section_title
;
 Crippling the C70 Fullerene: Non-Classical C68Cl26(OH)2 and C68Cl25(OH)3
 with Three Heptagons and Only Fused Pentagons via Chlorination-Promoted
 Skeletal Transformations
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01719A
_journal_year                    2022
_chemical_formula_sum            'C89 H26.41 Cl25.58 O2.42'
_chemical_formula_weight         2041.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2022-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                72.780(10)
_cell_angle_beta                 74.710(10)
_cell_angle_gamma                65.420(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3880(10)
_cell_length_b                   14.0840(10)
_cell_length_c                   22.734(2)
_cell_measurement_reflns_used    1500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      4
_cell_volume                     3674.4(6)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXD
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.799
_diffrn_measured_fraction_theta_max 0.602
_diffrn_measurement_device_type  Pilatus2M
_diffrn_measurement_method       HPC
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8266
_diffrn_reflns_av_R_equivalents  0.1751
_diffrn_reflns_av_unetI/netI     0.7192
_diffrn_reflns_Laue_measured_fraction_full 0.799
_diffrn_reflns_Laue_measured_fraction_max 0.602
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21417
_diffrn_reflns_point_group_measured_fraction_full 0.799
_diffrn_reflns_point_group_measured_fraction_max 0.602
_diffrn_reflns_theta_full        29.450
_diffrn_reflns_theta_max         36.930
_diffrn_reflns_theta_min         1.892
_diffrn_source                   'BL 14.2 PSF, BESSY, Berlin, Germany'
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       plate
_exptl_crystal_F_000             2030
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.801
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1032
_refine_ls_number_reflns         14265
_refine_ls_number_restraints     734
_refine_ls_restrained_S_all      0.788
_refine_ls_R_factor_all          0.4805
_refine_ls_R_factor_gt           0.1391
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0770P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.2568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2788
_reflns_number_total             14265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01719a2.cif
_cod_data_source_block           c70sb3f7
_cod_database_code               7130129
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              26682
_shelx_hkl_checksum              72709