An Unconventional Hydrofullerene C<sub>66</sub>H<sub>4</sub> with Symmetric Heptagons Retrieved in Low-Pressure Combustion.
Tian, Han-Rui; Chen, Miao-Miao; Wang, Kai; Chen, Zuo-Chang; Fu, Chao-Yong; Zhang, Qianyan; Li, Shu-Hui; Deng, Shun-Liu; Yao, Yang-Rong; Xie, Su-Yuan; Huang, Rong-Bin; Zheng, Lan-Sun; Journal of the American Chemical Society 141 (2019) 6651–6657; doi:10.1021/jacs.9b01638

data_4128243
_publ_section_title
;
 An Unconventional Hydrofullerene C<sub>66</sub>H<sub>4</sub> with
 Symmetric Heptagons Retrieved in Low-Pressure Combustion.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6651
_journal_page_last               6657
_journal_paper_doi               10.1021/jacs.9b01638
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C66 H4, C7 H8'
_chemical_formula_sum            'C73 H12'
_chemical_formula_weight         888.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                75.265(7)
_cell_angle_beta                 78.398(6)
_cell_angle_gamma                86.169(6)
_cell_formula_units_Z            4
_cell_length_a                   13.5363(9)
_cell_length_b                   15.7638(13)
_cell_length_c                   17.5101(13)
_cell_measurement_reflns_used    4487
_cell_measurement_temperature    100
_cell_measurement_theta_max      62.3640
_cell_measurement_theta_min      2.8990
_cell_volume                     3539.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     33.00  64.00   1.00    7.30    --    0.00  57.00-120.00   31
  2  \w    -22.00  10.00   1.00    7.30    --    0.00 -99.00 -30.00   32
  3  \w    -28.00   2.00   1.00    7.30    --    0.00  57.00-120.00   30
  4  \w    -25.00  31.00   1.00    7.30    --    0.00 -99.00  90.00   56
  5  \w    -98.00 -12.00   1.00    5.00    --  -48.75 -77.00 -60.00   86
  6  \w    -32.00  26.00   1.00    5.00    --  -48.75  77.00 -30.00   58
  7  \w    -73.00 -25.00   1.00    5.00    --  -48.75 126.00-180.00   48
  8  \w     33.00  89.00   1.00    5.00    --   48.75  57.00  30.00   56
  9  \w      1.00  95.00   1.00    5.00    --   48.75-126.00 150.00   94
 10  \w    -28.00  88.00   1.00    5.00    --   48.75 -38.00 120.00  116
 11  \w     21.00 121.00   1.00    5.00    --   48.75  57.00  60.00  100
 12  \w   -161.00-118.00   1.00   25.00    --  -92.00 -50.00 -90.00   43
 13  \w   -116.00 -90.00   1.00   25.00    --  -92.00 112.00 150.00   26
 14  \w    -41.00 -15.00   1.00   25.00    --  -92.00 112.00   0.00   26
 15  \w   -123.00 -88.00   1.00   25.00    --  -92.00 131.00 137.70   35
 16  \w   -157.00-131.00   1.00   25.00    --  -92.00 -92.00 -30.00   26
 17  \w     86.00 112.00   1.00   25.00    --   97.50 -92.00 -60.00   26
 18  \w     59.00 173.00   1.00   25.00    --   97.50  38.00   0.00  114
 19  \w     81.00 127.00   1.00   25.00    --   97.50 -64.00 150.00   46
 20  \w     20.00 142.00   1.00   25.00    --   97.50 -92.00-150.00  122
 21  \w     34.00  87.00   1.00   25.00    --   97.50-112.00  30.00   53
 22  \w     23.00  88.00   1.00   25.00    --   97.50-112.00-180.00   65
 23  \w     30.00  88.00   1.00   25.00    --   97.50-112.00  90.00   58
 24  \w     80.00 172.00   1.00   25.00    --   97.50  50.00 -60.00   92
 25  \w     20.00  67.00   1.00   25.00    --   97.50-112.00  60.00   47
 26  \w     35.00  60.00   1.00   25.00    --   97.50 -92.00 -60.00   25
 27  \w     61.00 149.00   1.00   25.00    --   97.50  38.00 -90.00   88
 28  \w     25.00  65.00   1.00   25.00    --   97.50-112.00-150.00   40
 29  \w     19.00  70.00   1.00   25.00    --   97.50-112.00 150.00   51
 30  \w     19.00  85.00   1.00   25.00    --   97.50-112.00 120.00   66
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0396351000
_diffrn_orient_matrix_UB_12      0.0703912000
_diffrn_orient_matrix_UB_13      0.0461212000
_diffrn_orient_matrix_UB_21      0.0284227000
_diffrn_orient_matrix_UB_22      -0.0599728000
_diffrn_orient_matrix_UB_23      0.0770492000
_diffrn_orient_matrix_UB_31      0.1054683000
_diffrn_orient_matrix_UB_32      0.0407733000
_diffrn_orient_matrix_UB_33      -0.0229136000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.1289
_diffrn_reflns_Laue_measured_fraction_full 0.867
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21499
_diffrn_reflns_point_group_measured_fraction_full 0.867
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         62.515
_diffrn_reflns_theta_min         2.658
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          4.0
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1357
_refine_ls_number_reflns         11084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.1094
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1213P)^2^+16.2755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3281
_refine_ls_wR_factor_ref         0.3511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6946
_reflns_number_total             11084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01638_si_002.cif
_cod_data_source_block           exp_17225
_cod_database_code               4128243
_shelxl_version_number           2014-1
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C140(0.5) H32(0.5) H30(0.5) H31(0.5) C142(0.5) H18(0.5) C143(0.5)
 H20(0.5) C144(0.5) H22(0.5) C145(0.5) H24(0.5) C146(0.5) H26(0.5) C141(0.5)
 C149(0.5) H17(0.5) C148(0.5) C153(0.5) H25(0.5) C152(0.5) H23(0.5) C151(0.5)
 H21(0.5) C150(0.5) H19(0.5) C147(0.5) H28(0.5) H27(0.5) H29(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C67(H5), C68(H6), C69(H7), C70(H8)
3.b Aromatic/amide H refined with riding coordinates:
 C135(H9), C136(H10), C137(H11), C138(H12), C139(H13), C142(H18), C143(H20),
 C144(H22), C145(H24), C146(H26), C149(H17), C153(H25), C152(H23), C151(H21),
 C150(H19)
3.c Fitted hexagon refined as free rotating group:
 C142(C143,C144,C145,C146,C141), C149(C148,C153,C152,C151,C150)
3.d Idealised Me refined as rotating group:
 C133(H14,H15,H16), C140(H32,H30,H31), C147(H28,H27,H29)
;
_shelx_res_checksum              63221
_shelx_hkl_checksum              1727
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.801
_oxdiff_exptl_absorpt_empirical_full_min 0.305