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_1566074
_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         'C86 H116 Au4 P4, C2 H2 Cl4'
_chemical_formula_sum            'C88 H118 Au4 Cl4 P4'
_chemical_formula_weight         2229.36
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-29
_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                 90.962(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7069(4)
_cell_length_b                   15.0274(3)
_cell_length_c                   16.9838(3)
_cell_measurement_reflns_used    11116
_cell_measurement_temperature    100.1(6)
_cell_measurement_theta_max      69.0380
_cell_measurement_theta_min      3.7260
_cell_volume                     4263.37(15)
_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      100.1(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.996
_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     44.00  69.00   1.00    0.30    --   45.53  70.00 -68.00   25
  2  \w     92.00 178.00   1.00    1.40    --   97.85  30.00-120.00   86
  3  \w    130.00 155.00   1.00    1.40    --   97.85  70.00 -68.00   25
  4  \w     22.00  51.00   1.00    1.40    --   97.85 -45.00-150.00   29
  5  \w     21.00  46.00   1.00    1.40    --   97.85 -45.00-180.00   25
  6  \w     21.00  46.00   1.00    1.40    --   97.85 -45.00   0.00   25
  7  \w     23.00  50.00   1.00    1.40    --   97.85 -45.00  60.00   27
  8  \w     23.00  86.00   1.00    1.40    --   97.85 -70.00 159.00   63
  9  \w     25.00  50.00   1.00    1.40    --   97.85 -45.00 150.00   25
 10  \w     21.00  46.00   1.00    1.40    --   97.85 -45.00  30.00   25
 11  \w     21.00  46.00   1.00    1.40    --   97.85 -45.00 -60.00   25
 12  \w     21.00  46.00   1.00    1.40    --   97.85 -45.00 -30.00   25
 13  \w     -1.00  24.00   1.00    0.30    --   45.53 -70.00 159.00   25
 14  \w   -154.00 -69.00   1.00    1.40    --  -95.66 -70.00 159.00   85
 15  \w   -102.00 -15.00   1.00    0.30    --  -43.34 -70.00 159.00   87
 16  \w    -74.00 -21.00   1.00    1.40    --  -95.66  70.00 -68.00   53
 17  \w    -51.00 -20.00   1.00    1.40    --  -95.66  45.00 -60.00   31
 18  \w   -104.00 -22.00   1.00    1.40    --  -95.66  77.00 120.00   82
 19  \w    -46.00 -20.00   1.00    1.40    --  -95.66  45.00 150.00   26
 20  \w    -91.00 -57.00   1.00    1.40    --  -95.66 125.00  60.00   34
 21  \w    -50.00 -21.00   1.00    1.40    --  -95.66  45.00-120.00   29
 22  \w    -67.00  31.00   1.00    0.30    --  -43.34  70.00 -68.00   98
 23  \w     27.00 104.00   1.00    1.40    --   97.85 -94.00   0.00   77
 24  \w   -102.00 -70.00   1.00    0.30    --  -43.34-125.00-120.00   32
 25  \w   -106.00 -78.00   1.00    0.30    --  -43.34-125.00 -90.00   28
 26  \w   -111.00 -70.00   1.00    0.30    --  -43.34-125.00 -60.00   41
 27  \w    -95.00 -70.00   1.00    1.40    --  -95.66-125.00 120.00   25
 28  \w   -169.00-129.00   1.00    1.40    --  -95.66-125.00 120.00   40
;
_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      -0.0241423000
_diffrn_orient_matrix_UB_12      0.0566306000
_diffrn_orient_matrix_UB_13      0.0713907000
_diffrn_orient_matrix_UB_21      0.0751924000
_diffrn_orient_matrix_UB_22      0.0580453000
_diffrn_orient_matrix_UB_23      -0.0101996000
_diffrn_orient_matrix_UB_31      -0.0477455000
_diffrn_orient_matrix_UB_32      0.0626262000
_diffrn_orient_matrix_UB_33      -0.0550238000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28905
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.999
_diffrn_reflns_theta_min         3.680
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52985
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       plate
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.607
_refine_diff_density_min         -2.016
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7392
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0924P)^2^+5.9504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5961
_reflns_number_total             7392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05459g2.cif
_cod_data_source_block           AucomplexforCM2P4P
_cod_database_code               1566074
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.756
_diffrn_oxdiff_digest_frames
;
01a91baf860ede3461d275638a03966e140119892de
;
_diffrn_oxdiff_digest_hkl
;
01b8191a20743f6486f5ad76ee90e14d2f4ae6
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C0AA_$1-C0AA
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C0AA) = Uanis(Cl00) = Uanis(C0AA) = Uanis(Cl2) = Uanis(Cl00) = Uanis(Cl2)
= Uanis(C4) = Uanis(C4) = Uanis(Cl1) = Uanis(Cl0A) = Uanis(Cl1) = Uanis(Cl0A)
4. Others
 Fixed Sof: Cl00(0.5) Cl1(0.5) Cl0A(0.5) C4(0.5) H4(0.5) Cl2(0.5) C0AA(0.5)
 H0AA(0.5)
5.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00L(H00L), C00R(H00R), C00V(H00V), C4(H4), C0AA(H0AA)
5.b Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00S(H00C,H00F), C00T(H00J,H00O), C00U(H00S,H00T), C00X(H00U,
 H00X), C00Y(H00Y,H), C00Z(H00Z,HA), C010(H01A,H01B), C011(H01C,H01D),
 C012(H01E,H01F), C013(H01G,H01H), C014(H01I,H01J), C015(H01K,H01L), C016(H01M,
 H01N), C017(H01O,H01P), C018(H01Q,H01R), C019(H01S,H01T), C01A(H01U,H01V),
 C01B(H01W,H01X), C01C(H01Y,HB), C01D(H01Z,HC)
5.c Aromatic/amide H refined with riding coordinates:
 C008(H008), C009(H009), C00D(H00D), C00E(H00E), C00G(H00G), C00I(H00I),
 C00K(H00K), C00M(H00M), C00N(H00N), C00P(H00P), C00Q(H00Q), C00W(H00W)
;
_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 2.371
_oxdiff_exptl_absorpt_empirical_full_min 0.562