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_4134242
_publ_section_title
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 Toward the synthesis of a highly strained hydrocarbon belt.
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_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00112
_journal_year                    2020
_chemical_formula_moiety         'C60 H80, C2 H4 Cl2'
_chemical_formula_sum            'C62 H84 Cl2'
_chemical_formula_weight         900.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-25
_audit_creation_method
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Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
????
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_cell_angle_alpha                90
_cell_angle_beta                 95.093(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.369(6)
_cell_length_b                   12.529(3)
_cell_length_c                   16.684(4)
_cell_measurement_reflns_used    7479
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4810
_cell_measurement_theta_min      1.2254
_cell_volume                     5282(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15732
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         1.814
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       prism
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4717
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1590P)^2^+9.7416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2780
_refine_ls_wR_factor_ref         0.2831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4370
_reflns_number_total             4717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00112_si_004.cif
_cod_data_source_block           mx6321d
_cod_database_code               4134242
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
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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. Restrained distances
 C17A-C16A = C16A-C15A = C18A-C17A
 1.54 with sigma of 0.01
 C24A-C23A = C22-C23A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C15A \\sim C16A \\sim C17A \\sim C18A \\sim C17 \\sim C18 \\sim C15 \\sim C16:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C23A \\sim C24A \\sim C23 \\sim C24: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq,
Uanis(C18A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C24A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(H16A)=
 Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=1-FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(C17)=Sof(H17C)=Sof(H17D)=Sof(C18)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=Sof(C15)=Sof(H15C)=Sof(H15D)=Sof(C16)=Sof(H16C)=Sof(H16D)=FVAR(1)
 Sof(H22C)=Sof(H22D)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=1-FVAR(2)
 Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23C)=Sof(H23D)=Sof(C24)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C14(H14C,H14D), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C22(H22C,H22D), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,H17B),
 C23A(H23A,H23B), C31(H31A,H31B), C23(H23C,H23D), C17(H17C,H17D), C15(H15C,
 H15D), C16(H16C,H16D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C9(H9), C12(H12)
5.d X=CH2 refined with riding coordinates:
 C29(H29A,H29B)
5.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C18A(H18A,H18B,
 H18C), C24A(H24A,H24B,H24C), C18(H18D,H18E,H18F), C24(H24D,H24E,H24F)
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_shelx_res_checksum              97531
_shelx_hkl_checksum              25451
_olex2_submission_special_instructions 'No special instructions were received'