Phenylene segments of zigzag carbon nanotubes synthesized by metal-mediated dimerization
Chen, Xuan-Wen; Chu, Ke-Shan; Wei, Rong-Jing; Qiu, Zhen-Lin; Tang, Chun; Tan, Yuan-Zhi; Chemical Science  (2022) –; doi:10.1039/D1SC05459G

data_1566078
_publ_section_title
;
 Phenylene segments of zigzag carbon nanotubes synthesized by
 metal-mediated dimerization
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05459G
_journal_year                    2022
_chemical_formula_moiety         '3(C S2), 4(C30 H20)'
_chemical_formula_sum            'C123 H80 S6'
_chemical_formula_weight         1750.23
_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             2021-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-06 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                74.817(2)
_cell_angle_beta                 83.098(2)
_cell_angle_gamma                82.344(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8159(2)
_cell_length_b                   18.1529(4)
_cell_length_c                   25.9016(5)
_cell_measurement_reflns_used    16576
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      65.3890
_cell_measurement_theta_min      2.5260
_cell_volume                     4844.88(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.975
_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    -66.00 -38.00   1.00    0.80    --  -41.86 102.00  92.00   28
  2  \w    -27.00   5.00   1.00    0.80    --  -41.86 102.00  92.00   32
  3  \w      7.00  88.00   1.00    0.80    --   43.42-102.00 -10.00   81
  4  \w    -75.00 -11.00   1.00    2.50    --  -89.37 102.00  92.00   64
  5  \w   -133.00-108.00   1.00    2.50    --  -89.37-102.00 -10.00   25
  6  \w     59.00 104.00   1.00    2.50    --   90.93-102.00 -10.00   45
  7  \w   -110.00 -84.00   1.00    0.80    --  -41.86-125.00  30.00   26
  8  \w    -42.00  38.00   1.00    0.80    --  -41.86  37.00  30.00   80
  9  \w    -96.00 -71.00   1.00    0.80    --  -41.86-125.00 150.00   25
 10  \w   -118.00 -71.00   1.00    0.80    --  -41.86-125.00 120.00   47
 11  \w    -38.00  20.00   1.00    0.80    --   43.42 -19.00  90.00   58
 12  \w    -39.00  -3.00   1.00    0.80    --   43.42 -19.00-180.00   36
 13  \w    -31.00  66.00   1.00    0.80    --   43.42 -57.00  30.00   97
 14  \w   -159.00-106.00   1.00    2.50    --  -89.37 -45.00  90.00   53
 15  \w    -35.00 -10.00   1.00    2.50    --  -89.37  30.00  60.00   25
 16  \w    -35.00 -10.00   1.00    2.50    --  -89.37  30.00 120.00   25
 17  \w    -51.00 -13.00   1.00    2.50    --  -89.37  45.00  60.00   38
 18  \w    -35.00  -9.00   1.00    2.50    --  -89.37  30.00-180.00   26
 19  \w    -60.00 -14.00   1.00    2.50    --  -89.37  61.00 120.00   46
 20  \w    -70.00 -18.00   1.00    2.50    --  -89.37  61.00-150.00   52
 21  \w    -35.00 -10.00   1.00    2.50    --  -89.37  30.00-150.00   25
 22  \w    -39.00 -13.00   1.00    2.50    --  -89.37  45.00  30.00   26
 23  \w   -149.00 -83.00   1.00    2.50    --  -89.37 -94.00  90.00   66
 24  \w    -34.00  -9.00   1.00    2.50    --  -89.37  30.00-120.00   25
 25  \w    -46.00 -14.00   1.00    2.50    --  -89.37 125.00  90.00   32
 26  \w     13.00  39.00   1.00    2.50    --   90.93 -45.00 -90.00   26
 27  \w     18.00  71.00   1.00    2.50    --   90.93 -61.00-150.00   53
 28  \w     63.00 104.00   1.00    2.50    --   90.93 -77.00  30.00   41
 29  \w     18.00  44.00   1.00    2.50    --   90.93 -77.00  30.00   26
 30  \w     15.00 109.00   1.00    2.50    --   90.93 -94.00   0.00   94
 31  \w     58.00 105.00   1.00    2.50    --   90.93 -77.00-150.00   47
 32  \w     28.00  54.00   1.00    2.50    --   90.93 -77.00-150.00   26
 33  \w     76.00 113.00   1.00    2.50    --   90.93-125.00 -60.00   37
 34  \w     63.00 154.00   1.00    2.50    --   90.93  61.00 -30.00   91
 35  \w    120.00 152.00   1.00    2.50    --   90.93  61.00  60.00   32
 36  \w     36.00  62.00   1.00    2.50    --   90.93-125.00 -60.00   26
 37  \w     16.00  48.00   1.00    2.50    --   90.93 -45.00-120.00   32
 38  \w     70.00 113.00   1.00    2.50    --   90.93  61.00  60.00   43
 39  \w     46.00  71.00   1.00    2.50    --   90.93 -61.00-180.00   25
 40  \w     93.00 152.00   1.00    2.50    --   90.93 125.00  90.00   59
 41  \w     51.00 102.00   1.00    2.50    --   90.93-125.00-180.00   51
 42  \w     32.00 116.00   1.00    2.50    --   90.93-125.00-150.00   84
 43  \w    112.00 137.00   1.00    2.50    --   90.93 102.00  92.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0013091000
_diffrn_orient_matrix_UB_12      0.0413156000
_diffrn_orient_matrix_UB_13      0.0448210000
_diffrn_orient_matrix_UB_21      0.0408792000
_diffrn_orient_matrix_UB_22      -0.0771672000
_diffrn_orient_matrix_UB_23      0.0388347000
_diffrn_orient_matrix_UB_31      0.1383718000
_diffrn_orient_matrix_UB_32      0.0126129000
_diffrn_orient_matrix_UB_33      -0.0176491000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54044
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.619
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       needle
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         16337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0992P)^2^+4.2028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13267
_reflns_number_total             16337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05459g2.cif
_cod_data_source_block           CM2P8P
_cod_database_code               1566078
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.823
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R), C00T(H00T),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C013(H013),
 C014(H014), C017(H017), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C),
 C01D(H01D), C01E(H01E), C01H(H01H), C01J(H01J), C01L(H01L), C01M(H01M),
 C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01S(H01S), C01T(H01T),
 C01U(H01U), C01W(H01W), C01X(H01X), C020(H020), C021(H021), C022(H022),
 C024(H024), C025(H025), C026(H026), C027(H027), C028(H028), C029(H029),
 C02A(H02A), C02E(H02E), C02G(H02G), C02H(H02H), C02J(H02J), C02K(H02K),
 C02M(H02M), C02N(H02N), C02P(H02P), C02R(H02R), C02S(H02S), C02T(H02T),
 C02U(H02U), C02V(H02V), C02W(H02W), C02Y(H02Y), C02Z(H02Z), C030(H030),
 C031(H031), C032(H032), C033(H033), C034(H034), C035(H035), C036(H036),
 C037(H037), C038(H038), C039(H039), C03A(H03A), C03B(H03B), C03C(H03C),
 C03D(H03D), C03E(H03E), C03F(H03F), C03G(H03G), C03H(H03H), C03I(H03I),
 C03J(H03J), C03K(H03K)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.009
_oxdiff_exptl_absorpt_empirical_full_min 0.481