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_1566076
_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         'C S2, C44 H28'
_chemical_formula_sum            'C45 H28 S2'
_chemical_formula_weight         632.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-23
_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                90
_cell_angle_beta                 111.135(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7656(10)
_cell_length_b                   5.8183(2)
_cell_length_c                   26.2196(12)
_cell_measurement_reflns_used    5161
_cell_measurement_temperature    99.8(6)
_cell_measurement_theta_max      71.4370
_cell_measurement_theta_min      3.6140
_cell_volume                     3239.4(3)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.953
_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     27.00  52.00   1.00    0.74    --   41.74  16.00  42.00   25
  2  \w     47.00 167.00   1.00    2.94    --  102.80  16.00  42.00  120
  3  \w     63.00 122.00   1.00    0.74    --   41.74 178.00 -60.00   59
  4  \w     31.00  69.00   1.00    2.94    --  102.80 -61.00 120.00   38
  5  \w     36.00  70.00   1.00    2.94    --  102.80 -61.00  90.00   34
  6  \w     25.00  50.00   1.00    2.94    --  102.80 -45.00  60.00   25
  7  \w     26.00  65.00   1.00    0.74    --   41.74 -57.00   0.00   39
  8  \w    -30.00  20.00   1.00    0.74    --   41.74 -57.00   0.00   50
  9  \w     25.00  50.00   1.00    2.94    --  102.80 -45.00 120.00   25
 10  \w     25.00  50.00   1.00    2.94    --  102.80 -45.00 -90.00   25
 11  \w     26.00  51.00   1.00    2.94    --  102.80 -45.00-120.00   25
 12  \w     26.00  51.00   1.00    2.94    --  102.80 -45.00  90.00   25
 13  \w     25.00  50.00   1.00    2.94    --  102.80 -45.00-150.00   25
 14  \w     33.00  62.00   1.00    2.94    --  102.80 -77.00-180.00   29
 15  \w     64.00 102.00   1.00    2.94    --  102.80 -77.00-180.00   38
 16  \w     67.00 115.00   1.00    2.94    --  102.80-125.00-150.00   48
 17  \w     31.00  56.00   1.00    2.94    --  102.80-125.00-150.00   25
 18  \w    -71.00 -46.00   1.00    2.94    --  -98.00  61.00 150.00   25
 19  \w     -1.00  41.00   1.00    0.74    --  -41.74  16.00  42.00   42
 20  \w    -68.00 -23.00   1.00    2.94    --  -98.00  61.00  90.00   45
 21  \w    -50.00 -24.00   1.00    2.94    --  -98.00  61.00-150.00   26
 22  \w    -70.00 -36.00   1.00    2.94    --  -98.00  61.00-180.00   34
 23  \w   -124.00   9.00   1.00    0.74    --  -41.74 -16.00-127.00  133
 24  \w   -128.00 -44.00   1.00    2.94    --  -98.00 -16.00-127.00   84
;
_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      0.0484117000
_diffrn_orient_matrix_UB_12      -0.0433455000
_diffrn_orient_matrix_UB_13      0.0578580000
_diffrn_orient_matrix_UB_21      0.0540375000
_diffrn_orient_matrix_UB_22      0.0386841000
_diffrn_orient_matrix_UB_23      -0.0213464000
_diffrn_orient_matrix_UB_31      0.0000255000
_diffrn_orient_matrix_UB_32      0.2582639000
_diffrn_orient_matrix_UB_33      0.0129043000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.908
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5306
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.490
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67795
_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    1.298
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0813
_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^)+(0.0482P)^2^+8.5685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1978
_refine_ls_wR_factor_ref         0.2039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4348
_reflns_number_total             5306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05459g2.cif
_cod_data_source_block           CN2P4P
_cod_depositor_comments
;

2022-09-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H56 S4'
_cod_original_formula_weight         1265.58
_cod_original_formula_moiety         '2(C S2), 2(C44 H28)'
_cod_original_formula_units_Z            2
_cod_database_code               1566076
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.724
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.591(5)
 0.409(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C8(H8), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25),
 C30(H30), C31(H31), C32(H32), C33(H33), C42(H42), C46(H46), C2(H2), C3(H3),
 C5(H5), C9(H9), C11(H11), C15(H15), C17(H17), C18(H18), C23(H23), C26(H26),
 C27(H27), C28(H28), C29(H29), C37(H37)
;
_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 1.675
_oxdiff_exptl_absorpt_empirical_full_min 0.478