Synthesis and Size-Dependent Properties of [12], [16], and [24]Carbon Nanobelts.
Povie, Guillaume; Segawa, Yasutomo; Nishihara, Taishi; Miyauchi, Yuhei; Itami, Kenichiro; Journal of the American Chemical Society 140 (2018) 10054–10059; doi:10.1021/jacs.8b06842

data_4132830
_publ_section_title
;
 Synthesis and Size-Dependent Properties of [12], [16], and [24]Carbon
 Nanobelts.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10054
_journal_page_last               10059
_journal_paper_doi               10.1021/jacs.8b06842
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'C64 H32, 0.5(C6 H14), 1.13(C6 H6), 1.13(C2 H Cl3)'
_chemical_formula_sum            'C76 H46.88 Cl3.38'
_chemical_formula_weight         1079.65
_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     dual
_audit_creation_date             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                88.1169(12)
_cell_angle_beta                 77.0096(12)
_cell_angle_gamma                71.8812(13)
_cell_formula_units_Z            4
_cell_length_a                   14.5888(2)
_cell_length_b                   17.7841(3)
_cell_length_c                   24.7553(3)
_cell_measurement_reflns_used    21828
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.8940
_cell_measurement_theta_min      2.4110
_cell_volume                     5943.27(16)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            80751
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.931
_diffrn_reflns_theta_min         1.887
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_correction_T_min  0.9904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2241
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.337
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1745
_refine_ls_number_reflns         25126
_refine_ls_number_restraints     894
_refine_ls_restrained_S_all      1.342
_refine_ls_R_factor_all          0.1735
_refine_ls_R_factor_gt           0.1122
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3374
_refine_ls_wR_factor_ref         0.3797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14257
_reflns_number_total             25126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06842_si_002.cif
_cod_data_source_block           16CNB
_cod_database_code               4132830
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.979
_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. Uiso/Uaniso restraints and constraints
C142 \\sim C143 \\sim C144 \\sim C145 \\sim C141 \\sim C146: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C163 \\sim C165 \\sim C166 \\sim C164 \\sim C161 \\sim C162: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Cl5 \\sim C149 \\sim C150 \\sim Cl4 \\sim Cl6 \\sim C160 \\sim C159 \\sim Cl19
\\sim Cl20 \\sim Cl21 \\sim Cl17 \\sim C157 \\sim C158 \\sim Cl16 \\sim Cl18
\\sim Cl8 \\sim C151 \\sim C152 \\sim Cl7 \\sim Cl9: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Cl1 \\sim C147 \\sim C148 \\sim Cl2 \\sim Cl3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Cl14 \\sim C155 \\sim C156 \\sim Cl13 \\sim Cl15: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
Cl6A \\sim C1M \\sim C1N \\sim Cl7A \\sim Cl8A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C154 \\sim C153 \\sim Cl10 \\sim Cl11 \\sim Cl12: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(C140) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C137) \\sim Ueq,
Uanis(C135) \\sim Ueq, Uanis(C138) \\sim Ueq, Uanis(C139) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C168) \\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(C167) \\sim Ueq,
Uanis(C170) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(C171) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(Cl1B)
\\sim Ueq, Uanis(Cl1C) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C1G) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1H)
\\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(C1F) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C144, C143, C142, C145, C141, C146, C166, C165, C164, C161, C163, C162
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl5, C149, C150, Cl4, Cl6, Cl17, C157, C158, Cl16, Cl18, C152, C151, Cl7, Cl8,
  Cl9, C160, C159, Cl19, Cl20, Cl21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3, C147, C148, Cl1, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl15, C155, C156, Cl13, Cl14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl6A, C1M, C1N, Cl7A, Cl8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C154, C153, Cl10, Cl11, Cl12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C168, C169, C167, C170, C172, C171
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C140, C136, C137, C135, C138, C139
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1A, C1A, C1B, Cl1B, Cl1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1F, C1C, C1D, C1H, C1E, C1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C165)=Sof(H165)=Sof(C166)=Sof(H166)=Sof(C161)=Sof(H161)=Sof(C162)=
 Sof(H162)=Sof(C163)=Sof(H163)=Sof(C164)=Sof(H164)=1-FVAR(1)
 Sof(C143)=Sof(H143)=Sof(C144)=Sof(H144)=Sof(C145)=Sof(H145)=Sof(C146)=
 Sof(H146)=Sof(C141)=Sof(H141)=Sof(C142)=Sof(H142)=FVAR(1)
 Sof(C168)=Sof(H168)=Sof(C169)=Sof(H169)=Sof(C170)=Sof(H170)=Sof(C171)=
 Sof(H171)=Sof(C172)=Sof(H172)=Sof(C167)=Sof(H167)=1-FVAR(2)
 Sof(C136)=Sof(H136)=Sof(C137)=Sof(H137)=Sof(C138)=Sof(H138)=Sof(C139)=
 Sof(H139)=Sof(C140)=Sof(H140)=Sof(C135)=Sof(H135)=FVAR(2)
 Fixed Sof: C159(0.25) C160(0.25) H160(0.25) Cl19(0.25) Cl20(0.25) Cl21(0.25)
 C153(0.25) C154(0.25) H154(0.25) Cl10(0.25) Cl11(0.25) Cl12(0.25) C147(0.25)
 C148(0.25) H148(0.25) Cl1(0.25) Cl2(0.25) Cl3(0.25) C157(0.25) C158(0.25)
 H158(0.25) Cl16(0.25) Cl17(0.25) Cl18(0.25) C1M(0.25) C1N(0.25) H1N(0.25)
 Cl6A(0.25) Cl7A(0.25) Cl8A(0.25) C151(0.25) C152(0.25) H152(0.25) Cl7(0.25)
 Cl8(0.25) Cl9(0.25) C149(0.25) C150(0.25) H150(0.25) Cl4(0.25) Cl5(0.25)
 Cl6(0.25) C155(0.25) C156(0.25) H156(0.25) Cl13(0.25) Cl14(0.25) Cl15(0.25)
 C1A(0.25) C1B(0.25) H1B(0.25) Cl1A(0.25) Cl1B(0.25) Cl1C(0.25) C1C(0.25)
 H1C(0.25) C1D(0.25) H1D(0.25) C1E(0.25) H1E(0.25) C1F(0.25) H1F(0.25)
 C1G(0.25) H1G(0.25) C1H(0.25) H1H(0.25)
5.a Free rotating group:
 C159(C160,Cl19,Cl20,Cl21), C153(C154,Cl10,Cl11,Cl12), C147(C148,Cl1,Cl2,Cl3),
 C157(C158,Cl16,Cl17,Cl18), C1M(C1N,Cl6A,Cl7A,Cl8A), C151(C152,Cl7,Cl8,Cl9),
 C149(C150,Cl4,Cl5,Cl6), C155(C156,Cl13,Cl14,Cl15), C1A(C1B,Cl1A,Cl1B,Cl1C),
 C1C(C1D,C1E,C1F,C1G,C1H)
5.b Secondary CH2 refined with riding coordinates:
 C134(H13A,H13B), C131(H13H,H13I), C133(H13C,H13D), C130(H13J,H13K)
5.c Aromatic/amide H refined with riding coordinates:
 C91(H91), C90(H90), C85(H85), C87(H87), C86(H86), C79(H79), C76(H76),
 C82(H82), C75(H75), C74(H74), C69(H69), C71(H71), C70(H70), C127(H127),
 C124(H124), C128(H128), C123(H123), C122(H122), C117(H117), C119(H119),
 C118(H118), C111(H111), C108(H108), C114(H114), C107(H107), C106(H106),
 C101(H101), C103(H103), C102(H102), C95(H95), C92(H92), C98(H98), C43(H43),
 C42(H42), C37(H37), C39(H39), C38(H38), C31(H31), C28(H28), C34(H34), C27(H27),
  C26(H26), C21(H21), C23(H23), C22(H22), C15(H15), C12(H12), C18(H18),
 C11(H11), C10(H10), C5(H5), C7(H7), C6(H6), C63(H63), C60(H60), C64(H64),
 C59(H59), C58(H58), C53(H53), C55(H55), C54(H54), C47(H47), C44(H44), C50(H50),
  C143(H143), C144(H144), C145(H145), C146(H146), C141(H141), C142(H142),
 C165(H165), C166(H166), C161(H161), C162(H162), C163(H163), C164(H164),
 C136(H136), C137(H137), C138(H138), C139(H139), C140(H140), C135(H135),
 C168(H168), C169(H169), C170(H170), C171(H171), C172(H172), C167(H167),
 C160(H160), C154(H154), C148(H148), C158(H158), C1N(H1N), C152(H152),
 C150(H150), C156(H156), C1B(H1B), C1C(H1C), C1D(H1D), C1E(H1E), C1F(H1F),
 C1G(H1G), C1H(H1H)
5.d Fitted hexagon refined as free rotating group:
 C143(C144,C145,C146,C141,C142), C165(C166,C161,C162,C163,C164), C136(C137,
 C138,C139,C140,C135), C168(C169,C170,C171,C172,C167)
5.e Idealised Me refined as rotating group:
 C132(H13E,H13F,H13G), C129(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'