Dimeric structures of ketones and esters in porous adaptive crystals of adamantane-containing macrocycle
Shinkawa, Shoyo; Kawahata, Masatoshi; Yamaguchi, Kentaro; Tominaga, Masahide; CrystEngComm 26 (2024) 5358–5363; doi:10.1039/D4CE00718B

data_7249302
_publ_section_title
;
 Dimeric structures of ketones and esters in porous adaptive crystals of
 adamantane-containing macrocycle
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5358
_journal_page_last               5363
_journal_paper_doi               10.1039/D4CE00718B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_sum            'C60.84 H58.15 Br4 N4 O9.3'
_chemical_formula_weight         1313.86
_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-2019/3
_audit_update_record
;
2024-06-24 deposited with the CCDC.	2024-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                67.421(4)
_cell_angle_beta                 88.195(5)
_cell_angle_gamma                85.102(4)
_cell_formula_units_Z            1
_cell_length_a                   10.7974(15)
_cell_length_b                   11.3923(16)
_cell_length_c                   12.1371(17)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.41
_cell_measurement_theta_min      3.94
_cell_volume                     1373.5(3)
_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-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.941
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20610
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.571
_diffrn_reflns_theta_min         3.944
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    4.094
_exptl_absorpt_correction_T_max  0.7716
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS G.M.Sheldrick 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.705
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5621
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0798P)^2^+5.7798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5241
_reflns_number_total             5621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00718b2.cif
_cod_data_source_block           1d
_cod_depositor_comments
'Adding full bibliography for 7249299--7249303.cif.'
_cod_original_formula_sum        'C60.84 H58.15 Br4 N4 O9.30'
_cod_database_code               7249302
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.639
_shelx_estimated_absorpt_t_max   0.735
_shelx_res_checksum              34914
_shelx_hkl_checksum              61819