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_1566075
_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         'C68 H44'
_chemical_formula_sum            'C68 H44'
_chemical_formula_weight         861.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 107.360(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.1646(4)
_cell_length_b                   6.47980(10)
_cell_length_c                   25.8994(5)
_cell_measurement_reflns_used    7356
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      74.3420
_cell_measurement_theta_min      2.5520
_cell_volume                     2909.58(10)
_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      99.9(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.948
_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     82.00 177.00   1.00    0.80    --  109.46  30.00 -30.00   95
  2  \w     99.00 148.00   1.00    0.80    --  109.46  61.00-120.00   49
  3  \w     88.00 136.00   1.00    0.80    --  109.46 151.00 -39.00   48
  4  \w     36.00  61.00   1.00    0.80    --  109.46 -61.00  90.00   25
  5  \w     39.00  66.00   1.00    0.80    --  109.46 -61.00  60.00   27
  6  \w     35.00  66.00   1.00    0.80    --  109.46 -61.00  30.00   31
  7  \w     38.00 101.00   1.00    0.80    --  109.46 -77.00-180.00   63
  8  \w     36.00  97.00   1.00    0.80    --  109.46 -94.00 -90.00   61
  9  \w     69.00  96.00   1.00    0.80    --  109.46-125.00 -60.00   27
 10  \w     95.00 131.00   1.00    0.80    --  109.46-151.00 -83.00   36
 11  \w     55.00  80.00   1.00    0.15    --   42.72-151.00 -83.00   25
 12  \w     78.00 113.00   1.00    0.80    --  109.46-122.00  77.00   35
 13  \w     35.00 117.00   1.00    0.80    --  109.46-125.00 120.00   82
 14  \w     34.00  95.00   1.00    0.15    --   42.72-122.00  77.00   61
 15  \w    -79.00 -54.00   1.00    0.80    --  -96.00 122.00 159.00   25
 16  \w    -81.00 -28.00   1.00    0.15    --  -42.72 122.00 159.00   53
 17  \w    -45.00 -20.00   1.00    0.80    --  -96.00  45.00  30.00   25
 18  \w    -50.00 -24.00   1.00    0.80    --  -96.00  45.00 -30.00   26
 19  \w    -49.00 -20.00   1.00    0.80    --  -96.00  45.00 -60.00   29
 20  \w    -50.00 -21.00   1.00    0.80    --  -96.00  45.00 -90.00   29
 21  \w    -90.00 -65.00   1.00    0.80    --  -96.00 151.00 -39.00   25
 22  \w    -25.00  37.00   1.00    0.15    --  -42.72  19.00 -30.00   62
 23  \w    -26.00  39.00   1.00    0.15    --  -42.72  19.00 -90.00   65
 24  \w   -100.00 -72.00   1.00    0.15    --  -42.72-122.00  77.00   28
 25  \w   -103.00 -78.00   1.00    0.15    --  -42.72-125.00 150.00   25
 26  \w   -108.00 -83.00   1.00    0.15    --  -42.72-151.00 -83.00   25
 27  \w   -110.00 -81.00   1.00    0.15    --  -42.72-125.00-120.00   29
 28  \w   -117.00 -84.00   1.00    0.15    --  -42.72-125.00-150.00   33
 29  \w   -142.00 -54.00   1.00    0.80    --  -96.00-151.00 -83.00   88
;
_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      0.0647828000
_diffrn_orient_matrix_UB_12      0.1137099000
_diffrn_orient_matrix_UB_13      0.0427284000
_diffrn_orient_matrix_UB_21      0.0407434000
_diffrn_orient_matrix_UB_22      -0.2074321000
_diffrn_orient_matrix_UB_23      0.0185704000
_diffrn_orient_matrix_UB_31      0.0451816000
_diffrn_orient_matrix_UB_32      0.0242288000
_diffrn_orient_matrix_UB_33      -0.0413781000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18828
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.336
_diffrn_reflns_theta_min         5.102
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66764
_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    0.983
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.047
_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     307
_refine_ls_number_reflns         5708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0672P)^2^+0.8823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4912
_reflns_number_total             5708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05459g2.cif
_cod_data_source_block           CN2P8P
_cod_database_code               1566075
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.939
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C004(H004), C005(H005), C006(H006), C009(H009), C00D(H00D), C00E(H00E),
 C00G(H00G), C00H(H00H), C00K(H00K), C00M(H00M), C00N(H00N), C00P(H00P),
 C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010)
;
_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 1.521
_oxdiff_exptl_absorpt_empirical_full_min 0.681