Quinoxaline-annelated hexadehydro[12]annulene: Use of a new building block to construct a hydrogen-bonded hexagonal molecular network
Kobayashi, Mayu; Kubo, Haruka; Oketani, Ryusei; Hisaki, Ichiro; CrystEngComm  (2022) –; doi:10.1039/D2CE00676F

data_7245099
_publ_section_title
;
 Quinoxaline-annelated hexadehydro[12]annulene: Use of a new building
 block to construct a hydrogen-bonded hexagonal molecular network
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00676F
_journal_year                    2022
_chemical_formula_moiety         'C72 H36 N6 O12, 4(C8 H8 O2), 0.5(C4 H9 O N)'
_chemical_formula_sum            'C106 H72.5 N6.5 O20.5'
_chemical_formula_weight         1765.27
_chemical_name_systematic
'hexakis(4-carboxyphenyl)triquinoxalinehexadehydro[12]annulene N,N-dimethylacetamide methyl benzoate solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-05-17 deposited with the CCDC.	2022-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.118(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            16
_cell_length_a                   49.9843(13)
_cell_length_b                   28.7291(6)
_cell_length_c                   26.9217(8)
_cell_measurement_reflns_used    7246
_cell_measurement_temperature    213
_cell_measurement_theta_max      67.87
_cell_measurement_theta_min      3.30
_cell_volume                     38439.5(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD Version 2013/2 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'PILATUS 200K/R'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1174
_diffrn_reflns_av_unetI/netI     0.1380
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            96948
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         74.416
_diffrn_reflns_theta_min         3.077
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             14688.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-dimethylacetamide, methyl benzoate'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1811
_refine_ls_number_reflns         37443
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1733
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2335
_refine_ls_wR_factor_ref         0.2855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14745
_reflns_number_total             37443
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d2ce00676f2.cif
_cod_data_source_block           TQ12-1(MeBz)
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C212 H145 N13 O41'
_cod_original_formula_weight         3530.54
_cod_original_formula_moiety         '2(C72 H36 N6 O12), 8(C8 H8 O2), C4 H9 O N'
_cod_original_formula_units_Z            8
_cod_database_code               7245099
_shelx_res_checksum              72102
_shelx_fab_checksum              48035