Structure analysis of inclusion crystals of diimide-based macrocycles with halocarbons
Tominaga, Masahide; Kondo, Sana; Hyodo, Tadashi; Kawahata, Masatoshi; Yamaguchi, Kentaro; CrystEngComm  (2022) –; doi:10.1039/D2CE00118G

data_7244673
_publ_section_title
;
 Structure analysis of inclusion crystals of diimide-based macrocycles
 with halocarbons
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00118G
_journal_year                    2022
_chemical_formula_sum            'C55 H47 Br9 N4 O8'
_chemical_formula_weight         1611.15
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-07 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                87.366(2)
_cell_angle_beta                 80.576(2)
_cell_angle_gamma                72.004(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8012(3)
_cell_length_b                   15.8268(4)
_cell_length_c                   18.8202(4)
_cell_measurement_reflns_used    28738
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.6810
_cell_measurement_theta_min      2.4840
_cell_volume                     2739.09(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (H\"ubschle et al., 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32381
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.440
_diffrn_reflns_theta_min         2.380
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    8.346
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.507
_refine_diff_density_min         -2.037
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10830
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1083P)^2^+22.5575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10016
_reflns_number_total             10830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00118g2.cif
_cod_data_source_block           2a
_cod_database_code               7244673
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.434
_shelx_estimated_absorpt_t_max   0.489
_shelx_res_checksum              2639
_shelx_hkl_checksum              7295