Capturing Nonclassical C70 with Double Heptagons in Low-Pressure Combustion
Xie, Fang-Fang; Chen, Zuo-Chang; Zhang, Min; Xie, Xiao-Ming; Chen, Ling-Fang; Tian, Hanrui; Deng, Shun-Liu; Xie, Su-Yuan; Zheng, Lansun; Chemical Communications  (2022) –; doi:10.1039/D2CC03707F

data_7130506
_publ_section_title
;
 Capturing Nonclassical C70 with Double Heptagons in Low-Pressure
 Combustion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03707F
_journal_year                    2022
_chemical_formula_moiety         '2(C60 H40 N10), C70 H6, 3(C7 H8), 1[C7H8]'
_chemical_formula_sum            'C218 H118 N20'
_chemical_formula_weight         3017.32
_chemical_name_systematic        dihept-C70H6
_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
_audit_creation_date             2022-08-02
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.07.25 svn.r36e0af09 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-08-03 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                78.553(3)
_cell_angle_beta                 77.136(2)
_cell_angle_gamma                70.866(3)
_cell_formula_units_Z            2
_cell_length_a                   14.8934(4)
_cell_length_b                   17.2624(5)
_cell_length_c                   30.2493(9)
_cell_measurement_reflns_used    16269
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      60.9010
_cell_measurement_theta_min      3.0080
_cell_volume                     7096.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     63.00 101.00   1.00    8.00    --   84.05-104.00-160.00   38
  2  \w    101.00 126.00   1.00    8.00    --   84.05 104.00 -59.00   25
  3  \w    -94.00 -20.00   1.00    8.00    --  -86.55 104.00 -59.00   74
  4  \w   -114.00 -85.00   1.00    8.00    --  -86.55-104.00-160.00   29
  5  \w    -17.00  29.00   1.00    2.00    --   -1.25 -99.00  90.00   46
  6  \w    -66.00   7.00   1.00    2.00    --   -1.25 -57.00  30.00   73
  7  \w      4.00  30.00   1.00    2.00    --   -1.25 -99.00-150.00   26
  8  \w    -10.00  68.00   1.00    2.00    --   -1.25  57.00-180.00   78
  9  \w    -13.00  24.00   1.00    2.00    --   -1.25 -99.00 -60.00   37
 10  \w     29.00  61.00   1.00    8.00    --   84.05 -57.00 -90.00   32
 11  \w     12.00  37.00   1.00    8.00    --   84.05 -38.00 -30.00   25
 12  \w     19.00  45.00   1.00    8.00    --   84.05 -38.00  90.00   26
 13  \w     12.00  55.00   1.00    8.00    --   84.05 -57.00   0.00   43
 14  \w     67.00 104.00   1.00    8.00    --   84.05 -99.00  30.00   37
 15  \w     69.00  99.00   1.00    8.00    --   84.05 -99.00  90.00   30
 16  \w     18.00  44.00   1.00    8.00    --   84.05 -38.00-120.00   26
 17  \w     15.00  40.00   1.00    8.00    --   84.05 -99.00  30.00   25
 18  \w     12.00  44.00   1.00    8.00    --   84.05 -38.00 -60.00   32
 19  \w     41.00 105.00   1.00    8.00    --   84.05 -77.00-150.00   64
 20  \w     16.00  45.00   1.00    8.00    --   84.05 -38.00   0.00   29
 21  \w     74.00 156.00   1.00    8.00    --   84.05  38.00  90.00   82
 22  \w     21.00  46.00   1.00    8.00    --   84.05 -99.00  90.00   25
 23  \w     48.00 105.00   1.00    8.00    --   84.05 -99.00 -30.00   57
 24  \w    -62.00 -35.00   1.00    8.00    --  -86.55  57.00   0.00   27
 25  \w   -110.00 -66.00   1.00    8.00    --  -86.55 125.00-180.00   44
 26  \w   -103.00 -22.00   1.00    8.00    --  -86.55  77.00 120.00   81
 27  \w    -98.00 -65.00   1.00    8.00    --  -86.55 -77.00 150.00   33
 28  \w    -40.00 -14.00   1.00    8.00    --  -86.55  38.00-120.00   26
 29  \w   -154.00-108.00   1.00    8.00    --  -86.55 -77.00 150.00   46
 30  \w    -41.00 -16.00   1.00    8.00    --  -86.55  38.00 -90.00   25
 31  \w   -106.00 -16.00   1.00    8.00    --  -86.55 125.00 150.00   90
 32  \w    -48.00 -14.00   1.00    8.00    --  -86.55 125.00-180.00   34
 33  \w    -65.00 -17.00   1.00    8.00    --  -86.55  77.00-180.00   48
 34  \w    -41.00 -16.00   1.00    8.00    --  -86.55  38.00-180.00   25
 35  \w    -54.00 -28.00   1.00    8.00    --  -86.55  77.00  60.00   26
 36  \w   -103.00 -60.00   1.00    8.00    --  -86.55  77.00  60.00   43
 37  \w    -98.00 -73.00   1.00    8.00    --  -86.55  77.00-180.00   25
 38  \w   -155.00 -83.00   1.00    8.00    --  -86.55 -19.00-120.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            75997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        61.169
_diffrn_reflns_theta_max         61.169
_diffrn_reflns_theta_min         2.735
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             3132
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2231
_refine_ls_number_reflns         21720
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1289P)^2^+7.5215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13412
_reflns_number_total             21720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03707f2.cif
_cod_data_source_block           exp_222_auto-r1
_cod_database_code               7130506
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.881
_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. Restrained planarity
 C0AA, C06O, C06N, C06E, C06M, C068, C065
 with sigma of 0.1
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C8, C9, C10, C11, C15, C21, C29, C31, C33, C40, C44,
 C60, C92, C94
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5AA, C2AA, C3AA, C7, C4AA, C1AA, C6AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C058, C05E, C05F, C05H, C05Y, C064, C06P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4AA, C5AA, C1AA, C3AA, C7, C2AA, C6AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C8 \\sim C9 \\sim C10
\\sim C11 \\sim C15 \\sim C21 \\sim C29 \\sim C31 \\sim C33 \\sim C40 \\sim C44
\\sim C60 \\sim C92 \\sim C94: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C5AA \\sim C2AA \\sim C3AA \\sim C7 \\sim C4AA \\sim C1AA \\sim C6AA: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C064 \\sim C058 \\sim C05E \\sim C05F \\sim C05Y \\sim C06P \\sim C05H: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C4AA \\sim C5AA \\sim C1AA \\sim C3AA \\sim C7 \\sim C2AA \\sim C6AA: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C5AA) = Uanis(C2AA) = Uanis(C3AA) = Uanis(C4AA) = Uanis(C6AA) =
Uanis(C1AA) = Uanis(C7)
Uanis(C065) = Uanis(C06O) = Uanis(C0AA) = Uanis(C06N) = Uanis(C06E) =
Uanis(C06M) = Uanis(C068)
5. Others
 Fixed Sof: C02P(0.5) C045(0.5) C048(0.5) C052(0.5) C054(0.5) C056(0.5)
 C058(0.75) H058(0.75) C059(0.5) C05E(0.75) C05F(0.75) H05F(0.75) C05G(0.5)
 C05H(0.75) H05H(0.75) C05K(0.5) C05M(0.5) C05P(0.5) C05Q(0.5) C05R(0.5)
 C05T(0.5) C05Y(0.75) H05Y(0.75) C062(0.5) C063(0.5) C064(0.75) H064(0.75)
 C067(0.5) C06A(0.5) C06C(0.5) C06D(0.5) C06P(0.75) H06D(0.75) H06E(0.75)
 H06F(0.75) C1(0.5) C2(0.5) C3(0.5) C4(0.5) C5(0.5) C6(0.5) C8(0.5) C9(0.5)
 C10(0.5) C11(0.5) C15(0.5) C21(0.5) C29(0.5) C31(0.5) C33(0.5) C40(0.5)
 C44(0.5) C60(0.5) C92(0.5) C94(0.5) C3AA(0.25) C4AA(0.25) H4AA(0.25)
 C5AA(0.25) H5AA(0.25) C1AA(0.25) H1AA(0.25) C7(0.25) H7(0.25) C2AA(0.25)
 H2AA(0.25) C6AA(0.25) H6AA(0.25) H6AB(0.25) H6AC(0.25)
6.a Ternary CH refined with riding coordinates:
 C03I(H03I), C03W(H03W), C04P(H04P), C04X(H04X), C05A(H05A), C05D(H05D)
6.b Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00X(H00X),
 C00Y(H00Y), C011(H011), C013(H013), C014(H014), C017(H017), C018(H018),
 C019(H019), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F),
 C01G(H01G), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01Q(H01Q),
 C01S(H01S), C01T(H01T), C01V(H01V), C01X(H01X), C01Z(H01Z), C020(H020),
 C021(H021), C022(H022), C023(H023), C024(H024), C025(H025), C026(H026),
 C027(H027), C028(H028), C029(H029), C02A(H02A), C02B(H02B), C02D(H02D),
 C02F(H02F), C02H(H02H), C02L(H02L), C02N(H02N), C02R(H02R), C02S(H02S),
 C02T(H02T), C02U(H02U), C036(H036), C03A(H03A), C03C(H03C), C03D(H03D),
 C03G(H03G), C03L(H03L), C03P(H03P), C03Y(H03Y), C042(H042), C043(H043),
 C044(H044), C04A(H04A), C04C(H04C), C04D(H04D), C04G(H04G), C04Q(H04Q),
 C04U(H04U), C04Y(H04Y), C053(H053), C055(H055), C057(H057), C058(H058),
 C05B(H05B), C05C(H05C), C05F(H05F), C05H(H05H), C05I(H05I), C05J(H05J),
 C05L(H05L), C05N(H05N), C05O(H05O), C05S(H05S), C05U(H05U), C05V(H05V),
 C05X(H05X), C05Y(H05Y), C05Z(H05Z), C060(H060), C064(H064), C066(H066),
 C06N(H06N), C06E(H06G), C06M(H06M), C068(H068), C065(H065), C4AA(H4AA),
 C5AA(H5AA), C1AA(H1AA), C7(H7), C2AA(H2AA)
6.c Fitted hexagon refined as free rotating group:
 C06O(C06N,C06E,C06M,C068,C065), C3AA(C4AA,C5AA,C1AA,C7,C2AA)
6.d Idealised Me refined as rotating group:
 C069(H06A,H06B,H06C), C06P(H06D,H06E,H06F), C0AA(H0AA,H0AB,H0AC), C6AA(H6AA,
 H6AB,H6AC)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 96 electrons were 
found in a volume of 542\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 1[C7H8] per Formula Unit 
which account for 100 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78703
_shelx_hkl_checksum              68922
_shelx_fab_checksum              43944
_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
;