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_7244676
_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            'C51 H56.67 I N4 O8.33'
_chemical_formula_weight         985.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-11 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.124(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.087(3)
_cell_length_b                   16.027(3)
_cell_length_c                   16.477(3)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.44
_cell_measurement_theta_min      3.61
_cell_volume                     4588.5(14)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            67015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.219
_diffrn_reflns_theta_min         2.543
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    5.975
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2041
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         11.400
_refine_diff_density_min         -4.862
_refine_diff_density_rms         0.361
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         9739
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      2.184
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.1070
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4024
_refine_ls_wR_factor_ref         0.4062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9518
_reflns_number_total             9739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00118g2.cif
_cod_data_source_block           1a_without_SQUEEZE
_cod_original_cell_volume        4588.6(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7244676
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.381
_shelx_estimated_absorpt_t_max   0.586
_shelx_res_checksum              88935
_shelx_hkl_checksum              5510