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_4134244
_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         'C48 H56'
_chemical_formula_sum            'C48 H60'
_chemical_formula_weight         636.96
_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_primary     iterative
_audit_creation_date             2019-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                72.612(3)
_cell_angle_beta                 88.798(2)
_cell_angle_gamma                61.900(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7332(3)
_cell_length_b                   12.2075(4)
_cell_length_c                   16.3902(5)
_cell_measurement_reflns_used    9323
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.7280
_cell_measurement_theta_min      4.3280
_cell_volume                     1956.16(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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    -62.00  31.00   1.00    1.00    --  -40.81  57.00  30.00   93
  2  \w    -62.00  33.00   1.00    1.00    --  -40.81  38.00 -90.00   95
  3  \w      1.00  27.00   1.00    1.00    --   40.81 -99.00-180.00   26
  4  \w     17.00  65.00   1.00    1.00    --   40.81 -99.00 -60.00   48
  5  \w     41.00  84.00   1.00    1.00    --  112.00 -61.00-180.00   43
  6  \w     94.00 121.00   1.00    1.00    --  112.00 -61.00-180.00   27
  7  \w     84.00 113.00   1.00    1.00    --  112.00-111.00-150.00   29
  8  \w     72.00 106.00   1.00    1.00    --  112.00 -95.00-120.00   34
  9  \w     68.00 114.00   1.00    1.00    --  112.00-111.00 -30.00   46
 10  \w     87.00 114.00   1.00    1.00    --  112.00-111.00  30.00   27
 11  \w    101.00 141.00   1.00    1.00    --  112.00 -77.00  60.00   40
 12  \w     69.00 108.00   1.00    1.00    --  112.00 -95.00  60.00   39
 13  \w     36.00  92.00   1.00    1.00    --   40.81-125.00 150.00   56
 14  \w     33.00  59.00   1.00    1.00    --  112.00 -95.00  60.00   26
 15  \w     38.00  85.00   1.00    1.00    --  112.00 -77.00  60.00   47
 16  \w     40.00 116.00   1.00    1.00    --  112.00-111.00   0.00   76
 17  \w     39.00  65.00   1.00    1.00    --  112.00-111.00 -30.00   26
 18  \w     36.00  65.00   1.00    1.00    --  112.00-111.00  30.00   29
 19  \w     37.00 116.00   1.00    1.00    --  112.00-111.00 150.00   79
 20  \w    134.00 173.00   1.00    1.00    --  112.00  45.00  30.00   39
 21  \w    117.00 165.00   1.00    1.00    --  112.00  77.00 120.00   48
 22  \w    111.00 178.00   1.00    1.00    --  112.00 111.00 150.00   67
 23  \w    105.00 131.00   1.00    1.00    --  112.00  77.00  60.00   26
 24  \w     80.00 147.00   1.00    1.00    --  112.00  77.00 150.00   67
 25  \w    100.00 159.00   1.00    1.00    --  112.00 111.00 -90.00   59
 26  \w    121.00 156.00   1.00    1.00    --  112.00  94.00-137.00   35
 27  \w    104.00 167.00   1.00    1.00    --  112.00  45.00 -90.00   63
 28  \w     87.00 172.00   1.00    1.00    --  112.00  45.00-150.00   85
 29  \w     53.00 136.00   1.00    1.00    --  112.00 -45.00-180.00   83
 30  \w   -109.00 -16.00   1.00    1.00    --  -40.81 -38.00  90.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18503
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.877
_diffrn_reflns_theta_min         4.316
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8121
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.486
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0733P)^2^+0.8028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6993
_reflns_number_total             8121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00112_si_002.cif
_cod_data_source_block           exp_547
_cod_database_code               4134244
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C20
 1.33 with sigma of 0.01
 C19-C21
 1.46 with sigma of 0.01
 C43-C45
 1.33 with sigma of 0.01
 C44-C45
 1.46 with sigma of 0.01
3. Rigid bond restraints
 C19, C21
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0001
 C19, C20
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0001
 C43, C45
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0001
4.a Ternary CH refined with riding coordinates:
 C10(H10), C22(H22), C34(H34), C46(H46)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C23(H23A,H23B), C35(H35A,H35B), C47(H47A,H47B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C14(H14), C15(H15), C18(H18), C26(H26), C27(H27),
 C30(H30), C38(H38), C41(H41), C42(H42)
4.d X=CH2 refined with riding coordinates:
 C9(H9A,H9B), C20(H20A,H20B), C32(H32A,H32B), C45(H45A,H45B)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C48(H48A,
 H48B,H48C)
;
_shelx_res_checksum              15045
_shelx_hkl_checksum              82709
_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
;