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_4134246
_publ_section_title
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 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                91.66(3)
_cell_angle_beta                 97.12(3)
_cell_angle_gamma                114.55(3)
_cell_formula_units_Z            2
_cell_length_a                   15.004(3)
_cell_length_b                   15.137(3)
_cell_length_c                   16.382(3)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4582
_cell_measurement_theta_min      1.2577
_cell_volume                     3344.8(14)
_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 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45366
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         1.258
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.931
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         15192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.1050
_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^)+(0.0934P)^2^+2.1835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2500
_refine_ls_wR_factor_ref         0.2594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12838
_reflns_number_total             15192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00112_si_007.cif
_cod_data_source_block           mx6702_sq
_cod_original_cell_volume        3344.6(14)
_cod_database_code               4134246
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.984
_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.a Ternary CH refined with riding coordinates:
 C1(H1), C5(H5), C9(H9), C13(H13), C18(H18), C22(H22), C26(H26), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C51(H51A,H51B), C61(H61A,H61B), C71(H71A,H71B)
2.c Me refined with riding coordinates:
 C59(H59A,H59B,H59C)
2.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C11(H11), C15(H15), C20(H20), C24(H24), C28(H28), C32(H32),
 C34(H34), C36(H36), C38(H38), C44(H44), C46(H46), C48(H48), C54(H54), C56(H56),
  C58(H58), C64(H64), C66(H66), C68(H68)
2.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C)
;
_shelx_res_checksum              129
_shelx_hkl_checksum              44305
_shelx_fab_checksum              15155
_olex2_submission_special_instructions 'No special instructions were received'