Co-crystals built from macrocycles with pyromellitic diimides and naphthalene derivatives: transformation of a binary co-crystal solvate to a solvate through solvent exchange
Tominaga, Masahide; Kamada, Ryusei; Hyodo, Tadashi; Yamaguchi, Kentaro; CrystEngComm 27 (2025) 5003–5009; doi:10.1039/D5CE00462D

data_7250667
_publ_section_title
;
 Co-crystals built from macrocycles with pyromellitic diimides and
 naphthalene derivatives: transformation of a binary co-crystal solvate to
 a solvate through solvent exchange
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5003
_journal_page_last               5009
_journal_paper_doi               10.1039/D5CE00462D
_journal_volume                  27
_journal_year                    2025
_chemical_formula_sum            'C60 H58 Br2 N4 O12'
_chemical_formula_weight         1186.92
_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
;
2024-10-08 deposited with the CCDC.	2025-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                94.639(2)
_cell_angle_beta                 92.734(2)
_cell_angle_gamma                107.934(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7166(6)
_cell_length_b                   11.3692(7)
_cell_length_c                   24.7966(16)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.44
_cell_measurement_theta_min      3.61
_cell_volume                     2590.0(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
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_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
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_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 0.989
_diffrn_measured_fraction_theta_max 0.935
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
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_diffrn_reflns_point_group_measured_fraction_full 0.989
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_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.641
_diffrn_reflns_theta_min         1.793
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  0.9171
_exptl_absorpt_correction_T_min  0.8008
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            yellowish-brown
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.447
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_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+1.7499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10351
_reflns_number_total             10549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00462d2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7250664--7250669.cif.'
_cod_database_code               7250667
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_shelx_estimated_absorpt_t_min   0.747
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_shelx_res_checksum              67773