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_1566077
_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         '2(C S2), C68 H44, C60'
_chemical_formula_sum            'C130 H44 S4'
_chemical_formula_weight         1733.89
_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             2021-08-20
_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                 100.313(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9720(2)
_cell_length_b                   21.5606(4)
_cell_length_c                   15.2604(3)
_cell_measurement_reflns_used    8441
_cell_measurement_temperature    99.8(7)
_cell_measurement_theta_max      74.9630
_cell_measurement_theta_min      4.0680
_cell_volume                     3875.43(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_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      99.8(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.992
_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    -79.00  33.00   1.00    1.51    --  -42.72  92.00-172.00  112
  2  \w      3.00  46.00   1.00    1.51    --   42.72 -92.00  75.00   43
  3  \w   -128.00-101.00   1.00    6.02    --  -96.00 -92.00  75.00   27
  4  \w    -52.00 -25.00   1.00    6.02    --  -96.00  92.00-172.00   27
  5  \w     37.00 108.00   1.00    6.02    --  109.46 -92.00  75.00   71
  6  \w    102.00 152.00   1.00    6.02    --  109.46  92.00-172.00   50
  7  \w   -118.00 -83.00   1.00    1.51    --  -42.72-125.00-180.00   35
  8  \w   -114.00 -84.00   1.00    1.51    --  -42.72-125.00-150.00   30
  9  \w    -24.00  17.00   1.00    1.51    --  -42.72  19.00 -60.00   41
 10  \w   -100.00 -70.00   1.00    1.51    --  -42.72-125.00-120.00   30
 11  \w     10.00  41.00   1.00    1.51    --   42.72  89.00 -43.27   31
 12  \w    -90.00 -25.00   1.00    6.02    --  -96.00 125.00-180.00   65
 13  \w   -107.00 -67.00   1.00    6.02    --  -96.00 -77.00 120.00   40
 14  \w    -51.00 -19.00   1.00    6.02    --  -96.00  45.00   0.00   32
 15  \w   -170.00-142.00   1.00    6.02    --  -96.00 -77.00 120.00   28
 16  \w    -51.00 -19.00   1.00    6.02    --  -96.00  45.00 -60.00   32
 17  \w    -51.00 -26.00   1.00    6.02    --  -96.00  45.00  60.00   25
 18  \w    -71.00 -33.00   1.00    6.02    --  -96.00  61.00 -30.00   38
 19  \w    -50.00 -19.00   1.00    6.02    --  -96.00  45.00 120.00   31
 20  \w    -51.00 -19.00   1.00    6.02    --  -96.00  45.00 150.00   32
 21  \w    -71.00 -35.00   1.00    6.02    --  -96.00  61.00  30.00   36
 22  \w    -50.00 -25.00   1.00    6.02    --  -96.00  45.00-180.00   25
 23  \w    -50.00 -20.00   1.00    6.02    --  -96.00  45.00  30.00   30
 24  \w    -59.00 -21.00   1.00    6.02    --  -96.00  61.00-180.00   38
 25  \w     35.00  75.00   1.00    6.02    --  109.46 -77.00 120.00   40
 26  \w     36.00 104.00   1.00    6.02    --  109.46 -77.00-120.00   68
 27  \w     71.00 113.00   1.00    6.02    --  109.46-125.00-120.00   42
 28  \w    131.00 172.00   1.00    6.02    --  109.46  45.00  90.00   41
 29  \w     98.00 128.00   1.00    6.02    --  109.46  45.00  90.00   30
 30  \w     78.00 105.00   1.00    6.02    --  109.46 -77.00 120.00   27
;
_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      -0.0299792000
_diffrn_orient_matrix_UB_12      -0.0437986000
_diffrn_orient_matrix_UB_13      -0.0805956000
_diffrn_orient_matrix_UB_21      0.0411660000
_diffrn_orient_matrix_UB_22      0.0492058000
_diffrn_orient_matrix_UB_23      -0.0601397000
_diffrn_orient_matrix_UB_31      0.1204616000
_diffrn_orient_matrix_UB_32      -0.0276728000
_diffrn_orient_matrix_UB_33      0.0204950000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25631
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.477
_diffrn_reflns_theta_min         3.587
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         6934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0568P)^2^+2.3071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5652
_reflns_number_total             6934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05459g2.cif
_cod_data_source_block           CN2P8PC60
_cod_database_code               1566077
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.923
_diffrn_oxdiff_digest_frames
;
0104ed196779a61e65aa7979ebe1f348e701197f414
;
_diffrn_oxdiff_digest_hkl
;
01ce5eecd7038591f6e16447eef5a3295c5eca
;
_reflns_odcompleteness_completeness 99.87
_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:
 C00A(H00A), C00B(H00B), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G),
 C00I(H00I), C00J(H00J), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O),
 C00Q(H00Q), C00R(H00R), 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 1.388
_oxdiff_exptl_absorpt_empirical_full_min 0.662