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_1566073
_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, C36 H24'
_chemical_formula_sum            'C37 H24 S2'
_chemical_formula_weight         532.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-17
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2609(8)
_cell_length_b                   17.4543(8)
_cell_length_c                   7.0890(3)
_cell_measurement_reflns_used    5884
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      31.0950
_cell_measurement_theta_min      3.0050
_cell_volume                     2630.69(19)
_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      100.0(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.822
_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    -26.00  12.00   0.50    5.00    --  -13.14 -99.00   0.00   76
  2  \w    -24.00  21.00   0.50    5.00    --  -13.14 -99.00-180.00   90
  3  \w    -26.00  25.00   0.50    5.00    --   14.55 -46.00 -84.00  102
  4  \w     12.00  62.00   0.50    5.00    --  -13.14  46.00  65.00  100
  5  \w     34.00  60.00   0.50    5.00    --  -13.14  57.00  90.00   52
;
_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      0.0163524000
_diffrn_orient_matrix_UB_12      -0.0270102000
_diffrn_orient_matrix_UB_13      -0.0565809000
_diffrn_orient_matrix_UB_21      0.0279021000
_diffrn_orient_matrix_UB_22      0.0219584000
_diffrn_orient_matrix_UB_23      0.0092025000
_diffrn_orient_matrix_UB_31      0.0081608000
_diffrn_orient_matrix_UB_32      -0.0209930000
_diffrn_orient_matrix_UB_33      0.0819964000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13166
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.184
_diffrn_reflns_theta_min         3.020
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45453
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       needle
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0596P)^2^+0.2164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2459
_reflns_number_total             3608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05459g2.cif
_cod_data_source_block           CM2P4P
_cod_depositor_comments
;

2022-09-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C148 H96 S8'
_cod_original_formula_weight         2130.72
_cod_original_formula_moiety         '4(C S2), 4(C36 H24)'
_cod_original_formula_units_Z            1
_cod_database_code               1566073
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.935
_diffrn_oxdiff_digest_frames
;
01cc75c74dab46f2aeb47334554ed146d60002763e2
;
_diffrn_oxdiff_digest_hkl
;
01d4b32e6af931974e2fd13bc3b5923bcfc626
;
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C006(H006), C008(H008), C00A(H00A), C00C(H00C), C00D(H00D),
 C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L)
;
_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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.474