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_1572863
_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, 5(C60), 7.2(C7 H8)'
_chemical_formula_sum            'C470.4 H161.6'
_chemical_formula_weight         5812.39
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2024-09-02 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   37.776(9)
_cell_length_b                   37.776(9)
_cell_length_c                   37.0120(12)
_cell_measurement_reflns_used    127027
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.3
_cell_volume                     45741(15)
_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_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(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 1.000
_diffrn_measured_fraction_theta_max 0.985
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            394855
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.416
_diffrn_reflns_theta_min         1.802
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.619
_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_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             17904
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 9212 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.12(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.352
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1857
_refine_ls_number_reflns         30067
_refine_ls_number_restraints     1743
_refine_ls_restrained_S_all      3.428
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.1680
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_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          0.4278
_refine_ls_wR_factor_ref         0.4423
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                23583
_reflns_number_total             30067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05938g3.cif
_cod_data_source_block           rk302ba
_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        45741(22)
_cod_original_formula_sum        'C470.40 H161.60'
_cod_database_code               1572863
_shelx_estimated_absorpt_t_min   0.907
_shelx_estimated_absorpt_t_max   0.921
_oxdiff_exptl_absorpt_empirical_full_min 0.775
_oxdiff_exptl_absorpt_empirical_full_max 1.346
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-2
_shelx_res_checksum              25307