Synthesis, crystal structure, and properties of methyl-substituted coronene amide analogue
Rakumitsu, Kenta; Fujii, Miho; Kusumoto, Sotaro; Kikkawa, Shoko; Azumaya, Isao; Yokoyama, Akihiro; RSC Advances 12 (2022) 26411–26417; doi:10.1039/D2RA04035B

data_7245506
_publ_section_title
;
 Synthesis, crystal structure, and properties of methyl-substituted
 coronene amide analogue
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              26411
_journal_page_last               26417
_journal_paper_doi               10.1039/D2RA04035B
_journal_volume                  12
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C36 H39 N3 O3'
_chemical_formula_sum            'C36 H39 N3 O3'
_chemical_formula_weight         561.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-12-25 deposited with the CCDC.	2022-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 116.5650(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.26590(10)
_cell_length_b                   25.57580(10)
_cell_length_c                   11.44520(10)
_cell_measurement_reflns_used    32191
_cell_measurement_temperature    93
_cell_measurement_theta_max      73.17
_cell_measurement_theta_min      3.46
_cell_volume                     2949.60(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39543
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.228
_diffrn_reflns_theta_min         3.456
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1200.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/n-hexane'
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details
;
 Flack x determined using 4678 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.55(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     823
_refine_ls_number_reflns         10360
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0773P)^2^+0.3718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                10048
_reflns_number_total             10360
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d2ra04035b2.cif
_cod_data_source_block           kkw_ayo210825_01_DCM-nHx
_cod_database_code               7245506
_shelx_res_checksum              51108