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_7244675
_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            'C57.5 H49.5 Cl4.5 N4 O10'
_chemical_formula_weight         1116.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 98.369(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0138(10)
_cell_length_b                   7.9580(3)
_cell_length_c                   27.4313(12)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.44
_cell_measurement_theta_min      3.61
_cell_volume                     5186.3(4)
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_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 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            60354
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.444
_diffrn_reflns_theta_min         2.644
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.855
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.8274
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+4.6133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7759
_reflns_number_total             10894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00118g2.cif
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C57.50 H49.50 Cl4.50 N4 O10'
_cod_database_code               7244675
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.804
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              97857
_shelx_hkl_checksum              22776