Pentacosacyclenes: cruciform molecular nanocarbons based on cyclooctatetraene.
Kumar, Rakesh; Chmielewski, Piotr J.; Lis, Tadeusz; Czarnecki, Mirosław; Stępień, Marcin; Chemical science 15 (2024) 18640–18649; doi:10.1039/d4sc05938g

data_1572861
_publ_section_title
;
 Pentacosacyclenes: cruciform molecular nanocarbons based on
 cyclooctatetraene.
;
_journal_issue                   44
_journal_name_full               'Chemical science'
_journal_page_first              18640
_journal_page_last               18649
_journal_paper_doi               10.1039/d4sc05938g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C120 H104, 6(C6 H14)'
_chemical_formula_sum            'C156 H188'
_chemical_formula_weight         2063.05
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-10-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-09-01 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.398(3)
_cell_length_b                   21.398(3)
_cell_length_c                   53.967(14)
_cell_measurement_reflns_used    25909
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      1.9
_cell_volume                     24710(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008'
_diffrn_ambient_temperature      80(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1481
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            194560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         1.903
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.109
_exptl_crystal_description       plate
_exptl_crystal_F_000             8992
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.614
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         7461
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.682
_refine_ls_R_factor_all          0.1883
_refine_ls_R_factor_gt           0.1132
_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^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2734
_refine_ls_wR_factor_ref         0.2976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3702
_reflns_number_total             7461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05938g3.cif
_cod_data_source_block           rk275ba
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1572861--1572863.cif.
;
_cod_original_cell_volume        24710(9)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               1572861
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Restrained distances
 C27-C28 = C27-C29 = C27-C29 = C27-C31 = C27-C32 = C27-C33
 1.52 with sigma of 0.01
 C41-C42 = C42-C43 = C43-C44 = C44-C45 = C45-C46
 1.52 with sigma of 0.015
 C41-C43 = C42-C44 = C43-C45 = C44-C46
 2.5 with sigma of 0.02
 C51-C52 = C52-C53 = C53-C54 = C54-C55 = C55-C56
 1.52 with sigma of 0.015
 C51-C53 = C52-C54 = C53-C55 = C54-C56
 2.5 with sigma of 0.02
 C81-C82 = C82-C83 = C83-C84 = C84-C85 = C85-C86
 1.52 with sigma of 0.015
 C81-C83 = C82-C84 = C83-C85 = C84-C86
 2.5 with sigma of 0.02
 C94-C95 = C95-C96 = C96-C96_$1
 1.52 with sigma of 0.015
 C94-C96 = C95-C96_$1
 2.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uiso(C41) = Uiso(C42) = Uiso(C43) = Uiso(C44) = Uiso(C45) = Uiso(C46)
Uiso(C71) = Uiso(C72) = Uiso(C73)
Uiso(C61) = Uiso(C62) = Uiso(C63)
Uiso(C51) = Uiso(C52) = Uiso(C53) = Uiso(C54) = Uiso(C55) = Uiso(C56)
Uiso(C81) = Uiso(C82) = Uiso(C83) = Uiso(C84) = Uiso(C85) = Uiso(C86)
Uiso(C91) = Uiso(C92) = Uiso(C93)
Uiso(C94) = Uiso(C95) = Uiso(C96)
3. Others
 Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5)
 H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C31(0.5) H31A(0.5)
 H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5) H33A(0.5)
 H33B(0.5) H33C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5) C45(0.5)
 H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C71(0.25)
 H71A(0.25) H71B(0.25) H71C(0.25) C72(0.25) H72A(0.25) H72B(0.25) C73(0.25)
 H73A(0.25) H73B(0.25) C61(0.25) H61A(0.25) H61B(0.25) H61C(0.25) C62(0.25)
 H62A(0.25) H62B(0.25) C63(0.25) H63A(0.25) H63B(0.25) C51(0.25) H51A(0.25)
 H51B(0.25) H51C(0.25) C52(0.25) H52A(0.25) H52B(0.25) C53(0.25) H53A(0.25)
 H53B(0.25) C54(0.25) H54A(0.25) H54B(0.25) C55(0.25) H55A(0.25) H55B(0.25)
 C56(0.25) H56A(0.25) H56B(0.25) H56C(0.25) C81(0.25) H81A(0.25) H81B(0.25)
 H81C(0.25) C82(0.25) H82A(0.25) H82B(0.25) C83(0.25) H83A(0.25) H83B(0.25)
 C84(0.25) H84A(0.25) H84B(0.25) C85(0.25) H85A(0.25) H85B(0.25) C86(0.25)
 H86A(0.25) H86B(0.25) H86C(0.25) C91(0.25) H91A(0.25) H91B(0.25) H91C(0.25)
 C92(0.25) H92A(0.25) H92B(0.25) C93(0.25) H93A(0.25) H93B(0.25) C94(0.25)
 H94A(0.25) H94B(0.25) H94C(0.25) C95(0.25) H95A(0.25) H95B(0.25) C96(0.25)
 H96A(0.25) H96B(0.25)
4.a Riding coordinates:
 C73(H73A,H73B), C93(H93A,H93B)
4.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C72(H72A,
 H72B), C62(H62A,H62B), C63(H63A,H63B), C52(H52A,H52B), C53(H53A,H53B),
 C54(H54A,H54B), C55(H55A,H55B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B),
  C85(H85A,H85B), C92(H92A,H92B), C95(H95A,H95B), C96(H96A,H96B)
4.c Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C46(H46A,H46B,H46C), C71(H71A,H71B,H71C), C61(H61A,H61B,
 H61C), C51(H51A,H51B,H51C), C56(H56A,H56B,H56C), C81(H81A,H81B,H81C), C86(H86A,
 H86B,H86C), C91(H91A,H91B,H91C), C94(H94A,H94B,H94C)
4.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9), C14(H14), C16(H16), C17(H17), C19(H19)
4.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              76568
_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 2.276
_oxdiff_exptl_absorpt_empirical_full_min 0.456