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_4134249
_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_absolute_configuration unk
_chemical_formula_moiety         'C76 H80, C2 H3 N'
_chemical_formula_sum            'C78 H83 N'
_chemical_formula_weight         1034.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 94.675(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.112(2)
_cell_length_b                   36.790(7)
_cell_length_c                   13.941(3)
_cell_measurement_reflns_used    18627
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4834
_cell_measurement_theta_min      1.4655
_cell_volume                     6703(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37710
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.200
_diffrn_reflns_theta_max         25.200
_diffrn_reflns_theta_min         1.465
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       plate
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 4667 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -3.7(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1470
_refine_ls_number_reflns         23047
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0930
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+3.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2301
_refine_ls_wR_factor_ref         0.2497
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.911
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                17921
_reflns_number_total             23047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00112_si_010.cif
_cod_data_source_block           mx6553b_sq
_cod_database_code               4134249
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.985
_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
 C52B-C50A = C51B-C50A = C52A-C50A = C51A-C50A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
H48A \\sim C50A \\sim C51A \\sim C52A \\sim C51B \\sim C52B: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
H32A \\sim C72A \\sim C74A \\sim C73A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C50A) \\sim Ueq, Uanis(C51A) \\sim Ueq, Uanis(C52A) \\sim Ueq,
Uanis(C51B) \\sim Ueq, Uanis(C52B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C72A) \\sim Ueq, Uanis(C74A) \\sim Ueq, Uanis(C73A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H50B)=Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52B)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=1-FVAR(1)
 Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52A)=Sof(H52A)=
 Sof(H52B)=Sof(H52C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C15(H15), C18(H18), C23(H23), C26(H26), C31(H31), C32(H32),
 C39(H39), C50(H50), C61(H61), C72(H72), C7A(H7A), C10A(H10A), C15A(H15A),
 C18A(H18A), C23A(H23A), C26A(H26A), C31A(H31A), C32A(H32A), C39A(H39A),
 C50A(H50A), C50A(H50B), C61A(H61A), C72A(H72A)
5.b Secondary CH2 refined with riding coordinates:
 C42(H42C,H42D), C53(H53C,H53D), C64(H64C,H64D), C75(H75C,H75D), C42A(H42A,
 H42B), C53A(H53A,H53B), C64A(H64A,H64B), C75A(H75A,H75B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C11(H11), C14(H14), C19(H19), C22(H22), C27(H27), C30(H30),
 C34(H34), C35(H35), C36(H36), C37(H37), C45(H45), C46(H46), C47(H47), C48(H48),
  C56(H56), C57(H57), C58(H58), C59(H59), C67(H67), C68(H68), C69(H69),
 C70(H70), C2A(H2A), C5A(H5A), C11A(H11A), C14A(H14A), C19A(H19A), C22A(H22A),
 C27A(H27A), C30A(H30A), C34A(H34A), C35A(H35A), C36A(H36A), C37A(H37A),
 C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A), C56A(H56A), C57A(H57A),
 C58A(H58A), C59A(H59A), C67A(H67A), C68A(H68A), C69A(H69A), C70A(H70A)
5.d Idealised Me refined as rotating group:
 C40(H40D,H40E,H40F), C41(H41D,H41E,H41F), C43(H43D,H43E,H43F), C51(H51G,H51H,
 H51I), C52(H52G,H52H,H52I), C54(H54D,H54E,H54F), C62(H62D,H62E,H62F), C63(H63D,
 H63E,H63F), C65(H65D,H65E,H65F), C73(H73D,H73E,H73F), C74(H74D,H74E,H74F),
 C76(H76D,H76E,H76F), C40A(H40A,H40B,H40C), C41A(H41A,H41B,H41C), C43A(H43A,
 H43B,H43C), C51A(H51A,H51B,H51C), C52A(H52A,H52B,H52C), C54A(H54A,H54B,H54C),
 C62A(H62A,H62B,H62C), C63A(H63A,H63B,H63C), C65A(H65A,H65B,H65C), C73A(H73A,
 H73B,H73C), C74A(H74A,H74B,H74C), C76A(H76A,H76B,H76C), C77(H77A,H77B,H77C),
 C79(H79A,H79B,H79C), C51B(H51D,H51E,H51F), C52B(H52D,H52E,H52F)
;
_shelx_res_checksum              72559
_shelx_hkl_checksum              51479
_shelx_fab_checksum              46783
_olex2_submission_special_instructions 'No special instructions were received'