Homo and Hetero Molecular 3D Nanographenes Employing a Cyclooctatetraene Scaffold.
Urieta-Mora, Javier; Krug, Marcel; Alex, Wiebke; Perles, Josefina; Fernandez, Israel; Molina-Ontoria, Agustín; Guldi, Dirk M.; Martín, Nazario; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10203

data_4134232
_publ_section_title
;
 Homo and Hetero Molecular 3D Nanographenes Employing a Cyclooctatetraene
 Scaffold.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10203
_journal_year                    2019
_chemical_formula_sum            'C108.88 H67.5 Cl0.5 O0.75'
_chemical_formula_weight         1405.35
_chemical_name_common            JU833_150K
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                93.006(5)
_cell_angle_beta                 96.297(5)
_cell_angle_gamma                104.808(5)
_cell_formula_units_Z            4
_cell_length_a                   20.3136(16)
_cell_length_b                   23.489(2)
_cell_length_c                   27.759(3)
_cell_measurement_reflns_used    9408
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      22.2100
_cell_measurement_theta_min      2.3075
_cell_volume                     12683(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1657
_diffrn_reflns_av_unetI/netI     0.1181
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            457936
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    0.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2941
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.415
_exptl_crystal_size_min          0.171
_refine_diff_density_max         2.320
_refine_diff_density_min         -1.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.760
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1911
_refine_ls_number_reflns         46468
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.761
_refine_ls_R_factor_all          0.4110
_refine_ls_R_factor_gt           0.2896
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3000P)^2^+19.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6505
_refine_ls_wR_factor_ref         0.7188
_reflns_number_gt                21388
_reflns_number_total             46468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10203_si_002.cif
_cod_data_source_block           6_02518AgustinMolina_vial2
_cod_original_cell_volume        12683.2(19)
_cod_original_formula_sum        'C108.88 H67.50 Cl0.50 O0.75'
_cod_database_code               4134232
_shelx_res_checksum              19483
_shelx_hkl_checksum              61110