Toward the synthesis of a highly strained hydrocarbon belt.
Shi, Tan-Hao; Guo, Qing-Hui; Tong, Shuo; Wang, Mei-Xiang; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00112

data_4134245
_publ_section_title
;
 Toward the synthesis of a highly strained hydrocarbon belt.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00112
_journal_year                    2020
_chemical_formula_moiety         'C72 H72'
_chemical_formula_sum            'C72 H72'
_chemical_formula_weight         937.29
_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             2019-11-23
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                75.021(2)
_cell_angle_beta                 88.6030(10)
_cell_angle_gamma                65.324(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5216(3)
_cell_length_b                   15.2767(3)
_cell_length_c                   17.1544(2)
_cell_measurement_reflns_used    33262
_cell_measurement_temperature    99.98(16)
_cell_measurement_theta_max      76.7390
_cell_measurement_theta_min      3.6280
_cell_volume                     3325.40(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -65.00  33.00   1.00    1.00    --  -40.81  38.00-120.00   98
  2  \w    -96.00  -2.00   1.00    1.00    --  -40.81 125.00 -30.00   94
  3  \w   -115.00 -16.00   1.00    1.00    --  -40.81 -38.00  60.00   99
  4  \w    -65.00  33.00   1.00    1.00    --  -40.81  38.00  60.00   98
  5  \w    -69.00  32.00   1.00    1.00    --  -40.81  57.00 -30.00  101
  6  \w     23.00  97.00   1.00    1.00    --   40.81-125.00-150.00   74
  7  \w     36.00 140.00   1.00    2.54    --  112.00 -30.00 -90.00  104
  8  \w     30.00 109.00   1.00    2.54    --  112.00 -95.00 -30.00   79
  9  \w     36.00 145.00   1.00    2.54    --  112.00 -77.00-180.00  109
 10  \w     36.00 140.00   1.00    2.54    --  112.00 -30.00 150.00  104
 11  \w     40.00 141.00   1.00    2.54    --  112.00 -61.00 120.00  101
 12  \w     30.00 109.00   1.00    2.54    --  112.00 -95.00 120.00   79
 13  \w     40.00 141.00   1.00    2.54    --  112.00 -61.00 -90.00  101
 14  \w     36.00 116.00   1.00    2.54    --  112.00-111.00-150.00   80
 15  \w     40.00 141.00   1.00    2.54    --  112.00 -61.00  30.00  101
 16  \w     36.00 116.00   1.00    2.54    --  112.00-111.00 -60.00   80
 17  \w     36.00 140.00   1.00    2.54    --  112.00 -30.00 150.00  104
 18  \w     79.00 178.00   1.00    2.54    --  112.00  77.00   0.00   99
 19  \w     36.00 140.00   1.00    2.54    --  112.00 -30.00  30.00  104
 20  \w     36.00 116.00   1.00    2.54    --  112.00-111.00  90.00   80
 21  \w     36.00 116.00   1.00    2.54    --  112.00-111.00 120.00   80
 22  \w     30.00 109.00   1.00    2.54    --  112.00 -95.00   0.00   79
 23  \w     40.00 141.00   1.00    2.54    --  112.00 -61.00-180.00  101
 24  \w     30.00 109.00   1.00    2.54    --  112.00 -95.00 150.00   79
 25  \w     36.00 116.00   1.00    2.54    --  112.00-111.00   0.00   80
 26  \w     36.00 116.00   1.00    2.54    --  112.00-111.00  60.00   80
 27  \w     24.00 178.00   1.00    2.54    --  112.00   0.00-180.00  154
 28  \w   -117.00  -8.00   1.00    1.00    --  -40.81 -77.00  30.00  109
 29  \w   -113.00 -13.00   1.00    1.00    --  -40.81 -57.00-180.00  100
 30  \w   -113.00 -13.00   1.00    1.00    --  -40.81 -57.00 -90.00  100
 31  \w    -65.00  33.00   1.00    1.00    --  -40.81  38.00 150.00   98
 32  \w      8.00 117.00   1.00    1.00    --   40.81  77.00  30.00  109
 33  \w      8.00 117.00   1.00    1.00    --   40.81  77.00 150.00  109
 34  \w      8.00 117.00   1.00    1.00    --   40.81  77.00 -90.00  109
 35  \w     83.00 178.00   1.00    2.54    --  112.00  61.00  90.00   95
 36  \w     83.00 178.00   1.00    2.54    --  112.00  61.00 -60.00   95
 37  \w     79.00 178.00   1.00    2.54    --  112.00  77.00 120.00   99
 38  \w     83.00 178.00   1.00    2.54    --  112.00  61.00  60.00   95
 39  \w     79.00 178.00   1.00    2.54    --  112.00  77.00-180.00   99
 40  \w     83.00 178.00   1.00    2.54    --  112.00  61.00 -30.00   95
 41  \w     79.00 178.00   1.00    2.54    --  112.00  77.00 150.00   99
 42  \w     59.00 178.00   1.00    2.54    --  112.00  15.00 -60.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0659584000
_diffrn_orient_matrix_UB_12      -0.0563015000
_diffrn_orient_matrix_UB_13      -0.0030343000
_diffrn_orient_matrix_UB_21      0.0862570000
_diffrn_orient_matrix_UB_22      -0.0980514000
_diffrn_orient_matrix_UB_23      0.0501932000
_diffrn_orient_matrix_UB_31      -0.0443167000
_diffrn_orient_matrix_UB_32      0.0229466000
_diffrn_orient_matrix_UB_33      0.0786945000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            82933
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.862
_diffrn_reflns_theta_min         3.577
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.936
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         13960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0515P)^2^+3.2838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12332
_reflns_number_total             13960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00112_si_009.cif
_cod_data_source_block           exp_1956_sq
_cod_database_code               4134245
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H71C)=Sof(H71D)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=1-FVAR(1)
 Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C28(H28), C25(H25), C7(H7), C10(H10), C62(H62), C46(H46), C61(H61), C43(H43)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C55(H55A,H55B), C19(H19A,H19B), C71(H71A,H71B), C71(H71C,H71D)
3.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C42(H42), C24(H24), C3(H3), C39(H39), C6(H6), C12(H12), C57(H57),
 C16(H16), C60(H60), C14(H14), C48(H48), C64(H64), C52(H52), C34(H34), C68(H68),
  C50(H50), C66(H66), C30(H30), C32(H32)
3.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C17(H17A,H17B,H17C), C56(H56A,H56B,H56C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C69(H69A,H69B,H69C), C54(H54A,H54B,H54C), C53(H53A,
 H53B,H53C), C70(H70A,H70B,H70C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C),
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              83312
_shelx_hkl_checksum              40803
_shelx_fab_checksum              64046
_platon_squeeze_void_probe_radius 1.20
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.756